Ammonia → HCID 67263977, 화합물

HRID 1687365노트

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HRID 1687365 반응식
[CH3:1][O:2][C:3]1[C:21]([N+:22]([O-:24])=[O:23])=[CH:20][C:6]2[N:7]([CH3:19])[C:8](=[O:18])[CH2:9][N:10](C(=O)C(F)(F)F)[CH2:11][C:5]=2[CH:4]=1.N>CO>[CH3:1][O:2][C:3]1[C:21]([N+:22]([O-:24])=[O:23])=[CH:20][C:6]2[N:7]([CH3:19])[C:8](=[O:18])[CH2:9][NH:10][CH2:11][C:5]=2[CH:4]=1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 86633916HCID 86633916, 화합물

생성물 1

HCID 67263977HCID 67263977, 화합물수율 77.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 7-Methoxy-1-methyl-8-nitro-4-(2,2,2-trifluoro-acetyl)-1,3,4,5-tetrahydro-benzo[e][1,4]diazepin-2-one (2.86 g, 0.00824 mol) and 7.0 M of Ammonia in Methanol (30 mL) were reacted in an analogous manner to example 736-D to give an oil. 7-Methoxy-1-methyl-8-nitro-1,3,4,5-tetrahydro[e][1,4]diazepin-2-one It was triturated with diethyl ether giving 7-Methoxy-1-methyl-8-nitro-1,3,4,5-tetrahydro-benzo[e][1,4]diazepin-2-one as a tan solid (1.61 g, 77%). Mp 145-149° C.; LCMS (m/e) 252 (M+1); 1H-NMR (DMSO, 400 MHz) δ 7.91 (s, 1H), 7.41 (s, 1H), 3.94 (s, 2H), 3.79 (s, 1H), 3.31 (s, 3H), 3.25 (s, 2H).

후처리

  1. customwere reacted in an analogous manner to example 736-D
  2. customto give an oil
  3. custom7-Methoxy-1-methyl-8-nitro-1,3,4,5-tetrahydro[e][1,4]diazepin-2-one It was triturated with diethyl ether

출처 및 근거

ORD 기록
ord-9116e04c57534f5492105a1f76f78bda
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148391B2

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