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

HRID 1258662노트

반응식

HRID 1258662 반응식
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

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 222Ammonia용매HCID 962Water용매HCID 8857Ethyl Acetate용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1f408d0685384336be2e90c87855920d
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08466186B2

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