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Water → 2-(2-Amino-pyrimidin-4-yl)-3-iodo-1-methyl-4-oxo-1,4,6,7-tetrahydro-pyrrolo[3,2-c]pyridine-5-carboxylic acid tert-butyl ester

HRID 869319
ノート
印刷プレビュー

反応式

HRID 869319 の反応式
[C:1](=O)([O-])[O-].[Cs+].[Cs+].[C:7]([O:11][C:12]([N:14]1[CH2:19][CH2:18][C:17]2[NH:20][C:21]([C:24]3[CH:29]=[CH:28][N:27]=[C:26]([NH2:30])[N:25]=3)=[C:22]([I:23])[C:16]=2[C:15]1=[O:31])=[O:13])([CH3:10])([CH3:9])[CH3:8].CI.O>CN(C=O)C.C(Cl)Cl>[C:7]([O:11][C:12]([N:14]1[CH2:19][CH2:18][C:17]2[N:20]([CH3:1])[C:21]([C:24]3[CH:29]=[CH:28][N:27]=[C:26]([NH2:30])[N:25]=3)=[C:22]([I:23])[C:16]=2[C:15]1=[O:31])=[O:13])([CH3:10])([CH3:8])[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 672844762-(2-Amino-pyrimidin-4-yl)-3-iodo-4-oxo-1,4,6,7-tetrahydro-pyrrolo[3,2-c]pyridine-5-carboxylic acid tert-butyl ester

生成物 1

HCID 672843262-(2-Amino-pyrimidin-4-yl)-3-iodo-1-methyl-4-oxo-1,4,6,7-tetrahydro-pyrrolo[3,2-c]pyridine-5-carboxylic acid tert-butyl ester収率 60%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

Cesium carbonate (2.17 g, 6.68 mmol) was added to a solution of 2-(2-amino-pyrimidin-4-yl)-3-iodo-4-oxo-1,4,6,7-tetrahydro-pyrrolo[3,2-c]pyridine-5-carboxylic acid tert-butyl ester (1.38 g, 3.03 mmol) in DMF (60 mL) and the mixture was stirred at room temperature for 1 h. Methyl iodide (0.948 g, 6.68 mmol) was then added and after 2 h stirring at room temperature, water (0.100 mL) and DCM (0.100 mL) were poured into the reaction vessel. The organic layer was separated, dried over Na2SO4, and concentrated under vacuum to yield the crude 2-(2-amino-pyrimidin-4-yl)-3-iodo-1-methyl-4-oxo-1,4,6,7-tetrahydro-pyrrolo[3,2-c]pyridine-5-carboxylic acid tert-butyl ester as a brown solid (0.854 g, 1.8 mmol, 60%).

後処理

  1. stirringstirring at room temperature
  2. customThe organic layer was separated
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-dc9a5f1a0a214579b8ba49dc9dc0e74b
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08969366B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート