HCID 59333282, 화합물 → HCID 59333338, 화합물

HRID 1893488노트

반응식

HRID 1893488 반응식
[CH2:1]([NH:8][C:9]1[CH:14]=[C:13]([N:15]2[CH:19]=[CH:18][N:17]=[CH:16]2)[C:12]([N+:20]([O-])=O)=[CH:11][C:10]=1[C:23]([F:26])([F:25])[F:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.O.[Sn](Cl)(Cl)(Cl)Cl>C(O)C>[CH2:1]([NH:8][C:9]1[CH:14]=[C:13]([N:15]2[CH:19]=[CH:18][N:17]=[CH:16]2)[C:12]([NH2:20])=[CH:11][C:10]=1[C:23]([F:26])([F:24])[F:25])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 59333282HCID 59333282, 화합물HCID 85782573Tin tetrachloride dihydrate

생성물 1

HCID 59333338HCID 59333338, 화합물수율 96.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of N-benzyl-5-(1H-imidazol-1-yl)-4-nitro-2-(trifluoromethyl)aniline (190 mg; 0.52 mmol; 1 eq) and tin chloride dihydrate (591 mg; 2.62 mmol; 5 eq) in ethanol (2 ml) is stirred under argon at 80° C. for 4 h. Concentration, partition (ethyl acetate/aqueous sodium hydrogenocarbonate), addition of solid sodium hydrogenocarbonate to adjust the pH around 8, filtration over Celite, extraction of the cake solid with ethyl acetate, reunion of the organic phases, additional washings (aqueous ammonium chloride, brine), drying (magnesium sulfate) and concentration affords the title product (165 mg; 0.50 mmol; 96%) as a yellow solid.

후처리

  1. concentrationConcentration
  2. custompartition
  3. addition(ethyl acetate/aqueous sodium hydrogenocarbonate), addition of solid sodium hydrogenocarbonate
  4. filtrationthe pH around 8, filtration
  5. extractionover Celite, extraction of the cake solid with ethyl acetate, reunion of the organic phases, additional washings (aqueous ammonium chloride, brine)
  6. customdrying
  7. concentration(magnesium sulfate) and concentration

출처 및 근거

ORD 기록
ord-c2001724a2614fefa0682d2a474a7731
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08513250B2

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