1,2-Dichloroethane → HCID 57194245, 화합물

HRID 496640노트

반응식

HRID 496640 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][C@H:10]([OH:13])[C@H:9]1[C:14]([OH:16])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl.[CH3:18][NH:19][O:20][CH3:21].C(Cl)CCl>CN(C1C=CN=CC=1)C.ClCCl>[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][C@H:10]([OH:13])[C@H:9]1[C:14](=[O:16])[N:19]([O:20][CH3:21])[CH3:18])=[O:7])([CH3:2])([CH3:3])[CH3:4]

참가 물질

6

반응물 3

HCID 111,2-DichloroethaneHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 14037017(2S,3S)-1-(tert-Butoxycarbonyl)-3-hydroxypyrrolidine-2-carboxylic acid

생성물 1

HCID 57194245HCID 57194245, 화합물수율 76.1%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

A mixture of compound 64 (8.42 g), N,O-dimethyl hydroxylamine HCl (10.66 g), DMAP (26.69 g), and EDC (10.47 g) in dichloromethane (500 ml) was stirred at ambient temperature for 16 hours. The reaction mixture was then applied directly to a silica flash column and eluted with ethyl acetate to give (2S,3S)-1-(tert-butoxycarbonyl)-3-hydroxy-2-(N-methoxy-N-methylcarbamoyl)pyrrolidine (compound 65) as a clear gum(7.6 g).

후처리

  1. washeluted with ethyl acetate

출처 및 근거

ORD 기록
ord-8e6da7377adb44b1911779e162c0a580
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06946468B1

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