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3,5-Bis(trifluoromethyl)benzylamine → HCID 23073257, 화합물

HRID 1157739
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HRID 1157739 반응식
[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
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참가 물질

5

반응물 3

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

생성물 1

HCID 23073257HCID 23073257, 화합물수율 83%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-650b7f08e3b54d85b70f5ef008584858
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07807701B2

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