Acetaldehyde → HCID 19418793, 화합물

HRID 2395739노트

반응식

HRID 2395739 반응식
C([BH3-])#N.[Na+].[CH3:5][C:6]([CH3:24])([O:8][C:9]([N:11]1[CH2:16][CH2:15][N:14]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[NH2:23])[CH2:13][CH2:12]1)=[O:10])[CH3:7].[CH:25](=O)[CH3:26]>CO>[CH3:7][C:6]([CH3:24])([O:8][C:9]([N:11]1[CH2:16][CH2:15][N:14]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[NH:23][CH2:25][CH3:26])[CH2:13][CH2:12]1)=[O:10])[CH3:5]

참가 물질

5

반응물 3

HCID 177AcetaldehydeHCID 2795530tert-Butyl 4-(2-aminophenyl)piperazine-1-carboxylateHCID 5003444Sodium cyanoborohydride

생성물 1

HCID 19418793HCID 19418793, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium cyanoborohydride (1.6 g) is added to a 0° solution of 1-[1,1-dimethylethoxycarbonyl]-4-(2-aminophenyl)piperazine (PREPARATION 13, 6.52 g) and acetaldehyde (1.48 ml) dissolved in methanol (65 ml). After 3 hr the reaction mixture is partially concentrated under reduced pressure. Then it is diluted with chloroform, washed with saturated aqueous sodium bicarbonate, saline, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give the title compound, Rf =0.62 (ethyl acetate/hexane, 1/1), NMR (300 MHz, CDCl3) 7.04, 6.95, 6.66, 4.59, 3.70-3.50, 3.15, 2.82, 1.49 and 1.28 δ.

후처리

  1. concentrationAfter 3 hr the reaction mixture is partially concentrated under reduced pressure
  2. additionThen it is diluted with chloroform
  3. washwashed with saturated aqueous sodium bicarbonate, saline
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-8d05a3171c8a4229abd5e08750d91be4
출처 데이터셋
uspto-grants-1996_02
특허 번호
US05489593

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