Lithium Hydroxide → 4-[(Benzyl)-(2,2,2-trichloro-ethoxycarbonyl)-amino]-pyrrolidine-1,2-dicarboxylicacid 1-tert-butyl ester

HRID 490576노트

반응식

HRID 490576 반응식
C[O:2][C:3]([CH:5]1[CH2:9][CH:8]([N:10]([CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:11]([O:13][CH2:14][C:15]([Cl:18])([Cl:17])[Cl:16])=[O:12])[CH2:7][N:6]1[C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])=[O:4].[Li+].[OH-]>CO>[C:29]([O:28][C:26]([N:6]1[CH2:7][CH:8]([N:10]([CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:11]([O:13][CH2:14][C:15]([Cl:16])([Cl:17])[Cl:18])=[O:12])[CH2:9][CH:5]1[C:3]([OH:4])=[O:2])=[O:27])([CH3:32])([CH3:30])[CH3:31]

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 675466644-[(Benzyl)-(2,2,2-trichloro-ethoxycarbonyl)-amino]-pyrrolidine-1,2-dicarboxylicacid 1-tert-butyl ester 2-methyl ester

생성물 1

HCID 675477354-[(Benzyl)-(2,2,2-trichloro-ethoxycarbonyl)-amino]-pyrrolidine-1,2-dicarboxylicacid 1-tert-butyl ester

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 4-[(benzyl)-(2,2,2-trichloro-ethoxycarbonyl)-amino]-pyrrolidine-1,2-dicarboxylicacid 1-tert-butyl ester 2-methyl ester in MeOH, cooled to 0 degree is added LiOH, and the mixture is stirred overnight. After removal of the solvent, the residue is acidified with HCl. The aqueous layer is extracted with EA, and the organic solution is dried, concentrated and purified to afford 4-[(benzyl)-(2,2,2-trichloro-ethoxycarbonyl)-amino]-pyrrolidine-1,2-dicarboxylicacid 1-tert-butyl ester (20).

후처리

  1. customAfter removal of the solvent
  2. extractionThe aqueous layer is extracted with EA
  3. customthe organic solution is dried
  4. concentrationconcentrated
  5. custompurified

출처 및 근거

ORD 기록
ord-cfe7702d6c4843d98a063c6bc7f4f16d
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07528136B2

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