Dichloromethane → HCID 44220300, 화합물

HRID 237382

반응식

HRID 237382 반응식
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]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 10796Cesium carbonateHCID 706072-Bromoethyldiethylammonium bromideHCID 44220298HCID 44220298, 화합물

생성물 1

HCID 44220300HCID 44220300, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
-140 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b99ec7c7e4ed4765b80750c6bbcafd16
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642594B2

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