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Water → (1S)-5-(1-Methyl-6-oxo-4-pyridin-4-yl-1,6-dihydro-pyrimidin-2-yl)-2,5-diaza-bicyclo[2.2.1]heptane-2-carboxylic acid tert-butyl ester

HRID 1348578
ノート
印刷プレビュー

反応式

HRID 1348578 の反応式
C(N(CC)CC)C.Cl.Cl[C:10]1[N:15]([CH3:16])[C:14](=[O:17])[CH:13]=[C:12]([C:18]2[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=2)[N:11]=1.[C:24]([O:28][C:29]([N:31]1[CH2:36][CH:35]2[CH2:37][C@H:32]1[CH2:33][NH:34]2)=[O:30])([CH3:27])([CH3:26])[CH3:25].O>CN(C)C=O>[C:24]([O:28][C:29]([N:31]1[CH2:36][CH:35]2[CH2:37][C@H:32]1[CH2:33][N:34]2[C:10]1[N:15]([CH3:16])[C:14](=[O:17])[CH:13]=[C:12]([C:18]2[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=2)[N:11]=1)=[O:30])([CH3:27])([CH3:25])[CH3:26]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 230245272-chloro-3-methyl-6-pyridin-4-yl-3H-pyrimidin-4-one hydrochlorideHCID 66592084(1S,4S)-(-)-2-Boc-2,5-diazabicyclo[2.2.1]heptane

生成物 1

HCID 68801880(1S)-5-(1-Methyl-6-oxo-4-pyridin-4-yl-1,6-dihydro-pyrimidin-2-yl)-2,5-diaza-bicyclo[2.2.1]heptane-2-carboxylic acid tert-butyl ester収率 72.1%

試薬・触媒・溶媒

1
HCID 6228Dimethylformamide溶媒

反応条件

温度
20 °C

実験手順

A mixture containing 10.7 ml (78.14 mmol) of triethylamine, 13.6 g (52.7 mmol) of 2-chloro-3-methyl-6-pyridin-4-yl-3H-pyrimidin-4-one hydrochloride (1:1), 6.0 g (30.24 mmol) of (1S)-2,5-diaza-bicyclo[2.2.1]heptane-2-carboxylic acid tert-butyl ester in 500 ml of anhydrous dimethylformamide is stirred at 20° C. for 6 h. Water is added to the cooled mixture and the resulting solution extracted with ethyl acetate. The combined extracts are washed with saturated aqueous ammonium chloride and saturated aqueous sodium chloride then-evaporated. The crude product is refluxed in diethylether for 1 h to afford 8.36 g of pure product as a brown solid.

後処理

  1. extractionthe resulting solution extracted with ethyl acetate
  2. washThe combined extracts are washed with saturated aqueous ammonium chloride and saturated aqueous sodium chloride
  3. customthen-evaporated
  4. temperatureThe crude product is refluxed in diethylether for 1 h

出典と根拠

ORDレコード
ord-0c65aa05e37f49ecb6cd4748622a6d81
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07211581B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート