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3,5-Bis(trifluoromethyl)benzylamine → HCID 23073257、化合物

HRID 1157739
ノート
印刷プレビュー

反応式

HRID 1157739 の反応式
[CH:1]1([CH2:6][N:7]([C:10]2[CH:18]=[C:17]3[C:13]([CH2:14][CH2:15][CH2:16]3)=[CH:12][C:11]=2[CH:19]=O)[CH2:8][CH3:9])[CH2:5][CH2:4][CH2:3][CH2:2]1.[F:21][C:22]([F:36])([F:35])[C:23]1[CH:24]=[C:25]([CH:28]=[C:29]([C:31]([F:34])([F:33])[F:32])[CH:30]=1)[CH2:26][NH2:27].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCl>[CH:1]1([CH2:6][N:7]([CH2:8][CH3:9])[C:10]2[CH:18]=[C:17]3[C:13](=[CH:12][C:11]=2[CH2:19][NH:27][CH2:26][C:25]2[CH:28]=[C:29]([C:31]([F:32])([F:33])[F:34])[CH:30]=[C:23]([C:22]([F:21])([F:35])[F:36])[CH:24]=2)[CH2:14][CH2:15][CH2:16]3)[CH2:5][CH2:4][CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 5210993,5-Bis(trifluoromethyl)benzylamineHCID 5049666Sodium triacetoxyborohydrideHCID 230732666-(N-cyclopentylmethyl-N-ethylamino)indane-5-carbaldehyde

生成物 1

HCID 23073257HCID 23073257、化合物収率 83%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution (20 ml) of 6-(N-cyclopentylmethyl-N-ethylamino)indane-5-carbaldehyde (1.09 g) and 3,5-bis(trifluoromethyl)benzylamine (1.26 g) in dichloromethane was added sodium triacetoxyborohydride (1.70 g) with stirring at room temperature. The reaction solution was stirred overnight. The reaction solution was washed successively with saturated aqueous sodium hydrogen carbonate, water and saturated brine, and the organic layer was dried over sodium sulfate. Sodium sulfate was filtered off and the filtrate was concentrated. The obtained residue was purified by column chromatography (n-hexane:ethyl acetate=6:1) to give the title compound (1.65 g, 83%).

後処理

  1. stirringThe reaction solution was stirred overnight
  2. washThe reaction solution was washed successively with saturated aqueous sodium hydrogen carbonate, water and saturated brine
  3. dry with materialthe organic layer was dried over sodium sulfate
  4. filtrationSodium sulfate was filtered off
  5. concentrationthe filtrate was concentrated
  6. customThe obtained residue was purified by column chromatography (n-hexane:ethyl acetate=6:1)

出典と根拠

ORDレコード
ord-650b7f08e3b54d85b70f5ef008584858
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07807701B2

反応ノート

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