Stannous chloride dihydrate → 1-(4,5-Diamino-2-chloro-phenyl)-pyrrolidine-3-carbonitrile

HRID 1258662ノート

反応式

HRID 1258662 の反応式
O.O.[Sn](Cl)Cl.[NH2:6][C:7]1[C:8]([N+:21]([O-])=O)=[CH:9][C:10]([Cl:20])=[C:11]([N:13]2[CH2:17][CH2:16][CH:15]([C:18]#[N:19])[CH2:14]2)[CH:12]=1>CCOC(C)=O.O.N>[NH2:21][C:8]1[C:7]([NH2:6])=[CH:12][C:11]([N:13]2[CH2:17][CH2:16][CH:15]([C:18]#[N:19])[CH2:14]2)=[C:10]([Cl:20])[CH:9]=1

参加物

6

反応物 2

HCID 61436Stannous chloride dihydrateHCID 679578281-(5-Amino-2-chloro-4-nitro-phenyl)-pyrrolidine-3-carbonitrile

生成物 1

HCID 679576781-(4,5-Diamino-2-chloro-phenyl)-pyrrolidine-3-carbonitrile

試薬・触媒・溶媒 3

HCID 222Ammonia溶媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

Tin dichloride dihydrate (410 mg, 1.8 mmol) was added to 1-(5-amino-2-chloro-4-nitro-phenyl)-pyrrolidine-3-carbonitrile (100 mg, 0.4 mmol) in EtOAc (5 mL). The reaction mixture was stirred at reflux for 1.5 h, cooled, diluted with EtOAc and water and basified with conc. ammonia. The mixture was filtered through a pad of celite. The organic layer was dried over Na2SO4 and concentrated to give the sub-title compound.

後処理

  1. temperatureat reflux for 1.5 h
  2. temperaturecooled
  3. filtrationThe mixture was filtered through a pad of celite
  4. dry with materialThe organic layer was dried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-1f408d0685384336be2e90c87855920d
出典データセット
uspto-grants-2013_06
特許番号
US08466186B2

反応ノート

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