Carbon Dioxide → N-(2-dimethylaminoethyl)-2-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl)propionamide

HRID 51498ノート

反応式

HRID 51498 の反応式
[NH2:1][C:2]1[C:3]2[C:10]([C:11]3[CH:16]=[CH:15][C:14]([O:17][C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)=[CH:13][CH:12]=3)=[CH:9][N:8]([CH:24]([CH3:30])[C:25](OCC)=[O:26])[C:4]=2[N:5]=[CH:6][N:7]=1.[CH3:31][N:32]([CH3:36])[CH2:33][CH2:34][NH2:35].C(=O)=O>CO>[CH3:31][N:32]([CH3:36])[CH2:33][CH2:34][NH:35][C:25](=[O:26])[CH:24]([N:8]1[C:4]2[N:5]=[CH:6][N:7]=[C:2]([NH2:1])[C:3]=2[C:10]([C:11]2[CH:12]=[CH:13][C:14]([O:17][C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)=[CH:15][CH:16]=2)=[CH:9]1)[CH3:30]

参加物

5

反応物 3

HCID 280Carbon DioxideHCID 66053N,N-DimethylethylenediamineHCID 22736339ethyl 2-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]propionate

生成物 1

HCID 22736284N-(2-dimethylaminoethyl)-2-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl)propionamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of ethyl 2-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]propionate (425 mg), N,N-dimethylethylenediamine (2 ml) and methanol (20 ml) was boiled under reflux for 18 hours with the exclusion of carbon dioxide. The mixture was cooled and filtered, the filtrate was diluted with water (50 ml) and stirred with ether. The mixture was left standing for 18 hours and the solid which precipitated was collected by filtration, washed with water and then ether and dried to give N-(2-dimethylaminoethyl)-2-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl)propionamide, m.p. 163-164° C.

後処理

  1. temperatureThe mixture was cooled
  2. filtrationfiltered
  3. additionthe filtrate was diluted with water (50 ml)
  4. waitThe mixture was left
  5. customthe solid which precipitated
  6. filtrationwas collected by filtration
  7. washwashed with water
  8. dry with materialether and dried

出典と根拠

ORDレコード
ord-491ecddd74694791a56ba0b52cd34afe
出典データセット
uspto-grants-2004_03
特許番号
US06713474B2

反応ノート

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