Methanamine, N-methoxy-, hydrochloride (1:1) → benzyl (2R,4R)-4-(tert-butyl-diphenyl-silanyloxy)-2-(methoxy-methyl-carbamoyl)-pyrrolidine-1-carboxylate

HRID 13432노트

반응식

HRID 13432 반응식
Cl.CN(C)CCCN=C=NCC.Cl.[CH3:14][O:15][NH:16][CH3:17].[CH2:18]([O:25][C:26]([N:28]1[CH2:32][C@H:31]([O:33][Si:34]([C:47]([CH3:50])([CH3:49])[CH3:48])([C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[CH2:30][C@@H:29]1[C:51]([OH:53])=O)=[O:27])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>N1C=CC=CC=1>[C:47]([Si:34]([C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)([C:41]1[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=1)[O:33][C@H:31]1[CH2:32][N:28]([C:26]([O:25][CH2:18][C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)=[O:27])[C@@H:29]([C:51](=[O:53])[N:16]([O:15][CH3:14])[CH3:17])[CH2:30]1)([CH3:48])([CH3:49])[CH3:50]

참가 물질

5

반응물 3

HCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 67482921(2R,4R)-4-(tert-butyl-diphenyl-silanyloxy)-pyrrolidine-1,2-dicarboxylic acid 1-benzyl ester

생성물 1

HCID 86619216benzyl (2R,4R)-4-(tert-butyl-diphenyl-silanyloxy)-2-(methoxy-methyl-carbamoyl)-pyrrolidine-1-carboxylate

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

1.50 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 761 mg of O,N-dimethylhydroxylamine hydrochloride were added in order to a pyridine (30 ml) solution of 2.62 g of (2R,4R)-4-(tert-butyl-diphenyl-silanyloxy)-pyrrolidine-1,2-dicarboxylic acid 1-benzyl ester obtained in (step 1), and the reaction liquid was stirred overnight at room temperature. The solvent of the reaction liquid was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1) to obtain the entitled compound.

후처리

  1. customobtained in (step 1)
  2. customthe reaction liquid
  3. customThe solvent of the reaction liquid
  4. customwas evaporated away under reduced pressure
  5. customthe resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=1/1)
  6. customto obtain the entitled compound

출처 및 근거

ORD 기록
ord-b3c821c278c449e8b0db555f13fb3e83
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

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