Lawesson's reagent → HCID 23366702、化合物
反応式
[S:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][NH:4][C:3](=O)[CH2:2]1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:22])=CC=1>C1(C)C=CC=CC=1>[S:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][NH:4][C:3](=[S:22])[CH2:2]1参加物
4
反応条件
- 温度
- 100 °C
実験手順
A stirred mixture of 4,5-dihydro-1,4-benzothiazepin-3(2H)-one (1.79 g, prepared as example 1 of international patent application WO 92/21668) and Lawesson's reagent (2.22 g) in dry toluene (100 ml) was heated at 100° C. for three hours. The mixture was allowed to cool to room temperature. The precipitated solid was collected by filtration, washed with toluene and dried to give 4,5-dihydro-1,4-benzothiazepin-3(2H)-thione. Yield 1.78 g (m.p. 215°-219° C.).
後処理
- temperatureto cool to room temperature
- filtrationThe precipitated solid was collected by filtration
- washwashed with toluene
- customdried
出典と根拠
- ORDレコード
- ord-7310f321071e48f4845a14ce9814a9d4
- 出典データセット
- uspto-grants-1996_12
- 特許番号
- US05580866
反応ノート
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