Aluminium lithium hydride → HCID 21262654、化合物

HRID 567750ノート

反応式

HRID 567750 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[CH:9]=[C:10]([CH:26]=[CH:27][CH:28]=1)[NH:11][C:12]1[C:13]2[CH:20]=[C:19]([C:21](OCC)=[O:22])[NH:18][C:14]=2[N:15]=[CH:16][N:17]=1>O>[Cl:7][C:8]1[CH:9]=[C:10]([CH:26]=[CH:27][CH:28]=1)[NH:11][C:12]1[C:13]2[CH:20]=[C:19]([CH2:21][OH:22])[NH:18][C:14]=2[N:15]=[CH:16][N:17]=1

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 212626224-(3-chloroanilino)-6-ethoxycarbonyl-7H-pyrrolo[2,3-d]pyrimidine

生成物 1

HCID 21262654HCID 21262654、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

Under a N2 atmosphere, 1.4 g (37 mmol) of lithium aluminum hydride are added in portions to 5.70 g (18 mmol) of 4-(3-chloroanilino)-6-ethoxycarbonyl-7H-pyrrolo[2,3-d]pyrimidine. After stirring at 50° C. for 2 h, 100 ml of water are added dropwise to the reaction mixture and it is filtered through Celite. Water is added to the filtrate and the mixture is extracted 3 times with ethyl acetate. The organic phases are washed 3 times with water and brine, dried (MgSO4) and evaporated. Recrystallization from isopropanol yields 4-(3-chloroanilino)-6-hydroxymethyl-7H-pyrrolo[2,3-d]pyrimidine; HPLC: tRet(Grad20)=8.2; TLC-Rf=0.11 (CH2Cl2/methanol [10:1]); MS: (M)+=274.

後処理

  1. filtrationis filtered through Celite
  2. additionWater is added to the filtrate
  3. extractionthe mixture is extracted 3 times with ethyl acetate
  4. washThe organic phases are washed 3 times with water and brine
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customRecrystallization from isopropanol

出典と根拠

ORDレコード
ord-2904ed77ba07439482a02ec12d983f52
出典データセット
uspto-grants-2001_01
特許番号
US06180636B2

反応ノート

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