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Water → HCID 10871416, 화합물

HRID 726867
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HRID 726867 반응식
[CH3:1][C:2]([CH3:11])([CH3:10])[C:3](=O)[C:4]([O:6]CC)=O.[C:12]1([C@@H:18]([NH2:20])[CH3:19])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.O>C1(C)C(C)=CC=CC=1>[CH3:11][C:2]([CH3:1])([CH3:10])[C:3](=[N:20][C@H:18]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[CH3:19])[C:4]([NH:20][C@H:18]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[CH3:19])=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 758181-Phenethylamine, (-)-HCID 220085Ethyl 3,3-dimethyl-2-oxobutanoate

생성물 1

HCID 10871416HCID 10871416, 화합물수율 45%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

A solution of 15 g (95 mmol) of ethyl trimethyl-pyruvate and 50 g (413 mmol) of (S)-1-phenylethylamine in 50 ml of xylene was boiled under reflux on a water separator for 18 hours. Subsequently, the solvent was distilled off and excess amine was removed at 120° C. in a vacuum. After crystallization of the distillation residue from 125 ml of hexane there were obtained 14.3 g (45%) of (S)-3,3-dimethyl-N-[(S)-1-phenylethyl]-2-(1-phenylethylimino)-butyramide of melting point 96°-97° C. [α]=-58.9 (c=1.0, CHCl3).

후처리

  1. distillationSubsequently, the solvent was distilled off
  2. customexcess amine was removed at 120° C. in a vacuum
  3. customAfter crystallization of the distillation residue from 125 ml of hexane

출처 및 근거

ORD 기록
ord-23ba930ea1634e12816ffa93b230c82e
출처 데이터셋
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05710322

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