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

HRID 490576ノート

反応式

HRID 490576 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-cfe7702d6c4843d98a063c6bc7f4f16d
出典データセット
uspto-grants-2009_05
特許番号
US07528136B2

反応ノート

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