benzyl 2-chloro-4-[5-chloro-4-(2-methyl-3-oxo-2,3-dihydro-1H-isoindol-4-yloxy)-pyrimidin-2-ylamino]-5-methoxy-benzoate → 2-chloro-4-[5-chloro-4-(2-methyl-3-oxo-2,3-dihydro-1H-isoindol-4-yloxy)-pyrimidin-2-ylamino]-5-methoxy-benzoic acid

HRID 81356ノート

反応式

HRID 81356 の反応式
[Cl:1][C:2]1[CH:17]=[C:16]([NH:18][C:19]2[N:24]=[C:23]([O:25][C:26]3[CH:34]=[CH:33][CH:32]=[C:31]4[C:27]=3[C:28](=[O:36])[N:29]([CH3:35])[CH2:30]4)[C:22]([Cl:37])=[CH:21][N:20]=2)[C:15]([O:38][CH3:39])=[CH:14][C:3]=1[C:4]([O:6]CC1C=CC=CC=1)=[O:5]>C1COCC1.C(#N)C.[OH-].[OH-].[Pd+2]>[Cl:1][C:2]1[CH:17]=[C:16]([NH:18][C:19]2[N:24]=[C:23]([O:25][C:26]3[CH:34]=[CH:33][CH:32]=[C:31]4[C:27]=3[C:28](=[O:36])[N:29]([CH3:35])[CH2:30]4)[C:22]([Cl:37])=[CH:21][N:20]=2)[C:15]([O:38][CH3:39])=[CH:14][C:3]=1[C:4]([OH:6])=[O:5]

参加物

5

反応物 1

HCID 58522534benzyl 2-chloro-4-[5-chloro-4-(2-methyl-3-oxo-2,3-dihydro-1H-isoindol-4-yloxy)-pyrimidin-2-ylamino]-5-methoxy-benzoate

生成物 1

HCID 585226292-chloro-4-[5-chloro-4-(2-methyl-3-oxo-2,3-dihydro-1H-isoindol-4-yloxy)-pyrimidin-2-ylamino]-5-methoxy-benzoic acid

試薬・触媒・溶媒 3

HCID 9942167Palladium hydroxide触媒HCID 6342Acetonitrile溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Benzyl 2-chloro-4-[5-chloro-4-(2-methyl-3-oxo-2,3-dihydro-1H-isoindol-4-yloxy)-pyrimidin-2-ylamino]-5-methoxy-benzoate (75 mg) is dissolved in THF (150 mL), Pd(OH)2 (0.01 g) is added and the mixture is stirred for 2 h under H2 gas. For working up the mixture is diluted with ACN (20 mL) and Isolute is added. The solvent is filtered off from the catalyst and the solvent is eliminated in vacuo.

後処理

  1. additionis added
  2. filtrationThe solvent is filtered off from the catalyst

出典と根拠

ORDレコード
ord-7583c66c6d484ecca2e2808a2873b164
出典データセット
uspto-grants-2014_09
特許番号
US08846689B2

反応ノート

読み込み中…