Ethanol → HCID 66851256, 화합물

HRID 37873노트

반응식

HRID 37873 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([N:9]2[CH2:15][CH2:14][CH2:13][N:12]([C:16]3[CH:21]=[CH:20][C:19]([N+:22]([O-])=O)=[CH:18][CH:17]=3)[CH2:11][CH2:10]2)[CH:3]=1.C(O)C.C(N(CC)CC)C>C(OCC)(=O)C>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([N:9]2[CH2:15][CH2:14][CH2:13][N:12]([C:16]3[CH:17]=[CH:18][C:19]([NH2:22])=[CH:20][CH:21]=3)[CH2:11][CH2:10]2)[CH:3]=1

참가 물질

5

반응물 3

HCID 702EthanolHCID 8471TriethylamineHCID 668515111-(4,6-Dimethyl-pyridin-2-yl)-4-(4-nitro-phenyl)-[1,4]diazepane

생성물 1

HCID 66851256HCID 66851256, 화합물수율 99.6%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 1-(4,6-dimethyl-pyridin-2-yl)-4-(4-nitro-phenyl)-[1,4]diazepane (940 mg, 2.88 mmol) in ethyl acetate (25 mL) was added stannous chloride (3.90 g, 17.3 mmol) and ethanol (5 mL). The reaction mixture was heated to reflux for 15 hours then cooled to room temperature, basified with triethylamine and filtered. The filtrate was concentrated under reduced pressure to afford 4-[4-(4,6-dimethyl-pyridin-2-yl)-[1,4]diazepan-1-yl]-phenylamine (850 mg, 99%) as a brown solid.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 15 hours
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-5d8f74c42ce14871b154b69129200291
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524705B2

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