10,11-Dihydro-11-oxodibenzo[b,f][1,4]thiazepine synthesis
- Product Name:10,11-Dihydro-11-oxodibenzo[b,f][1,4]thiazepine
- CAS Number:3159-07-7
- Molecular formula:C13H9NOS
- Molecular Weight:227.28
54920-98-8
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3159-07-7
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Yield:3159-07-7 86%
Reaction Conditions:
toluene-4-sulfonic acid in ethyl acetate;xylene at 125; for 10 h;
Steps:
3
Para-Toluene sulphonic acid (41 mg, 0.2175 mmol) was added to the ethyl acetate solution obtained in Example 2, and approx. 50% of the ethyl acetate was removed by distillation. Xylene (320 ml) was added to the reactor and the distillation was continued until a batch temperature of 125° C. was reached. The reaction was then heated for 10 hours with azeotropic removal of water. The vessel contents were cooled to 55° C. and the resulting suspension was filtered. The cake was washed with methanol (120 ml), isolated and dried in vacuo to give 10,11-dihydrodibenzo[b,f][1,4]thiazepin-11-one (28.4 g, 86%).
References:
Murray, Paul Michael;Vaz, Luis-Manuel;Ainge, Debra;Harada, Katsumasa;Nishino, Shigeyoshi;Yoshii, Kiyotaka US2007/203336, 2007, A1 Location in patent:Page/Page column 7
100866-62-4
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3159-07-7
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19806-43-0
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3159-07-7
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13739-55-4
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3159-07-7
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