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Potassium Carbonate → 1-[(3-Cyano-pyridin-2-yl)methyl]-3-methyl-7-(2-butyn-1-yl)-8-bromo-xanthine

HRID 424460
ノート
印刷プレビュー

反応式

HRID 424460 の反応式
[CH3:1][N:2]1[C:10]2[N:9]=[C:8]([Br:11])[N:7]([CH2:12][C:13]#[C:14][CH3:15])[C:6]=2[C:5](=[O:16])[NH:4][C:3]1=[O:17].C(=O)([O-])[O-].[K+].[K+].CN1CCCC1=O.Cl[CH2:32][C:33]1[C:38]([C:39]#[N:40])=[CH:37][CH:36]=[CH:35][N:34]=1>O>[C:39]([C:38]1[C:33]([CH2:32][N:4]2[C:5](=[O:16])[C:6]3[N:7]([CH2:12][C:13]#[C:14][CH3:15])[C:8]([Br:11])=[N:9][C:10]=3[N:2]([CH3:1])[C:3]2=[O:17])=[N:34][CH:35]=[CH:36][CH:37]=1)#[N:40]
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 11430Potassium CarbonateHCID 13387N-methyl-2-pyrrolidoneHCID 210889278-Bromo-7-(2-butyn-1-yl)-3,7-dihydro-3-methyl-1H-purine-2,6-dioneHCID 469118343-Pyridinecarbonitrile, 2-(chloromethyl)-

生成物 1

HCID 167265441-[(3-Cyano-pyridin-2-yl)methyl]-3-methyl-7-(2-butyn-1-yl)-8-bromo-xanthine

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

反応条件

温度
70 °C

実験手順

202 g (0.68 mol) 3-methyl-7-(2-butyn-1-yl)-8-bromo-xanthine, 188.5 g (1.36 mol) anhydrous potassium carbonate and 1.68 liters of N-methyl-2-pyrrolidone are placed in the reactor and heated to 70° C. Then 119 g (0.75 mol) 2-chloromethyl-3-cyano-pyridine in 240 ml N-methyl-2-pyrrolidine (NMP) are added dropwise. The contents of the reactor are stirred for 19 hours at 70° C. After the reaction has ended 2.8 liters of water are added to the reaction mixture and it is cooled to 25° C. The product is filtered off, washed with 2 liters of water and dried in the drying cupboard at 70° C. while being rendered inert.

後処理

  1. additionare added to the reaction mixture and it
  2. temperatureis cooled to 25° C
  3. filtrationThe product is filtered off
  4. washwashed with 2 liters of water
  5. customdried in the drying cupboard at 70° C.

出典と根拠

ORDレコード
ord-90b4fc25571942b19e005ee4a68026a8
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08106060B2

反応ノート

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