Methanol → (1S,2S)-(-)-1,2-diphenylethylenediamine.1-hydroxy-2-hydroxyimino-1,2-diphenylethane

HRID 1721506

반응식

HRID 1721506 반응식
[C:1]1([C@H:7]([NH2:16])[C@H:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[NH2:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CO.[OH:19][CH:20]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C:21](=[N:28][OH:29])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>C1C=CC=CC=1>[C:10]1([C@H:8]([NH2:9])[C@H:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[NH2:16])[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1.[OH:19][CH:20]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C:21](=[N:28][OH:29])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 9924(+-)-Benzoin oximeHCID 6931238(1S,2S)-1,2-diphenylethane-1,2-diamine

생성물 1

HCID 86749458(1S,2S)-(-)-1,2-diphenylethylenediamine.1-hydroxy-2-hydroxyimino-1,2-diphenylethane

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

0.934 g (4.40 mmol) of (1S,2S)-(-)-1,2-diphenylethylenediamine of α!D20 =-103.1° (c 1.00, MeOH ) and 1.00 g (4.40 mmol) of dl-1-hydroxy-2-hydroxyimino-1,2-diphenylethane were added to 3 ml of benzene and then heated and stirred, and the solution was cooled to room temperature. Afterward, the precipitated crystals were collected by filtration and then recrystallized from 2 ml of benzene once to obtain 0.250 g of (1S,2S)-(-)-1,2-diphenylethylenediamine·1-hydroxy-2-hydroxyimino-1,2-diphenylethane. Physical properties of the product are as follows.

후처리

  1. temperatureheated
  2. filtrationAfterward, the precipitated crystals were collected by filtration
  3. customrecrystallized from 2 ml of benzene once

출처 및 근거

ORD 기록
ord-a9601509502d433ba9f8767dcd2a28f4
출처 데이터셋
uspto-grants-1996_04
특허 번호
US05510520

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