Dichloromethane → HCID 44220300、化合物

HRID 237382ノート

反応式

HRID 237382 の反応式
C(=O)([O-])[O-].[Cs+].[Cs+].[CH2:7]([NH:9][C:10]([C:12]1[S:30][C:15]2[N:16]=[C:17]([NH2:29])[N:18]=[C:19]([C:20]3[CH:25]=[C:24]([OH:26])[C:23]([Cl:27])=[CH:22][C:21]=3[Cl:28])[C:14]=2[CH:13]=1)=[O:11])[CH3:8].ClCCl.Br.Br[CH2:36][CH2:37][N:38]([CH2:41][CH3:42])[CH2:39][CH3:40]>CN(C=O)C>[CH2:7]([NH:9][C:10]([C:12]1[S:30][C:15]2[N:16]=[C:17]([NH2:29])[N:18]=[C:19]([C:20]3[CH:25]=[C:24]([O:26][CH2:36][CH2:37][N:38]([CH2:41][CH3:42])[CH2:39][CH3:40])[C:23]([Cl:27])=[CH:22][C:21]=3[Cl:28])[C:14]=2[CH:13]=1)=[O:11])[CH3:8]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 10796Cesium carbonateHCID 706072-Bromoethyldiethylammonium bromideHCID 44220298HCID 44220298、化合物

生成物 1

HCID 44220300HCID 44220300、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
-140 °C

実験手順

Cesium carbonate was added to a solution of 2-Amino-4-(2,4-dichloro-5-hydroxyphenyl)-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl amide in DMF, 2-Bromo-N,N-diethylethylamine hydrobromide was added and the suspension heated, at −140° C., for ˜2 hrs. The resulting suspension was allowed to cool and dichloromethane added. The mixture was washed with water and saturated aqueous sodium chloride solution. The solution was dried over anhydrous sodium sulphate and concentrated to a dark brown gum. The crude product was purified by chromatography on silica eluting with mixtures of dichloromethane and methanol.

後処理

  1. additionwas added
  2. temperatureto cool
  3. washThe mixture was washed with water and saturated aqueous sodium chloride solution
  4. dry with materialThe solution was dried over anhydrous sodium sulphate
  5. concentrationconcentrated to a dark brown gum
  6. customThe crude product was purified by chromatography on silica eluting with mixtures of dichloromethane and methanol

出典と根拠

ORDレコード
ord-b99ec7c7e4ed4765b80750c6bbcafd16
出典データセット
uspto-grants-2014_02
特許番号
US08642594B2

反応ノート

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