HCID 59333282、化合物 → HCID 59333338、化合物

HRID 1893488ノート

反応式

HRID 1893488 の反応式
[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

参加物

4

反応物 2

HCID 59333282HCID 59333282、化合物HCID 85782573Tin tetrachloride dihydrate

生成物 1

HCID 59333338HCID 59333338、化合物収率 96.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c2001724a2614fefa0682d2a474a7731
出典データセット
uspto-grants-2013_08
特許番号
US08513250B2

反応ノート

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