Ethanol → HCID 66851256、化合物

HRID 37873ノート

反応式

HRID 37873 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 66851256HCID 66851256、化合物収率 99.6%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-5d8f74c42ce14871b154b69129200291
出典データセット
uspto-grants-2013_09
特許番号
US08524705B2

反応ノート

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