1H-1,5-Benzodiazepin-2-one, 2,3,4,5-tetrahydro-4-methyl- → 74389-71-2

HRID 1485476노트

반응식

HRID 1485476 반응식
[CH3:1][CH:2]1[CH2:8][C:7](=O)[NH:6][C:5]2[CH:10]=[CH:11][CH:12]=[CH:13][C:4]=2[NH:3]1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:23])=CC=1>C1COCC1>[CH3:1][CH:2]1[CH2:8][C:7](=[S:23])[NH:6][C:5]2[CH:10]=[CH:11][CH:12]=[CH:13][C:4]=2[NH:3]1

참가 물질

4

반응물 2

HCID 198681H-1,5-Benzodiazepin-2-one, 2,3,4,5-tetrahydro-4-methyl-HCID 87949Lawesson's reagent

생성물 1

HCID 303360874389-71-2수율 123.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
80 °C

실험 절차

A disposable tube was charged with 4-methyl-4,5-dihydro-1H-benzo[b][1,4]diazepin-2(3H)-one (220 mg, 1.248 mmol) in THF (12 mL). Lawesson's Reagent (278 mg, 0.687 mmol) was added, and the solution was stirred at 80° C. 1 h. The solution was concentrated with celite and purified by silica gel chromatography to yield 4-methyl-4,5-dihydro-1H-benzo[b][1,4]diazepine-2(3H)-thione as a yellow foam (0.163 g, 0.848 mmol, 68%).

후처리

  1. custom1 h
  2. concentrationThe solution was concentrated with celite
  3. custompurified by silica gel chromatography

출처 및 근거

ORD 기록
ord-a0b5cace1dc4446f97a87074f57d342c
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09422292B2

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