Hydrochloric Acid → HCID 59519252, 화합물

HRID 1161738노트

반응식

HRID 1161738 반응식
Cl.[CH2:2]([NH:4][C:5]([C:7]1[S:33][C:10]2[N:11]=[C:12]([NH2:32])[N:13]=[C:14]([C:15]3[CH:20]=[C:19]([O:21][CH2:22][CH:23](OCC)OCC)[C:18]([Cl:30])=[CH:17][C:16]=3[Cl:31])[C:9]=2[CH:8]=1)=[O:6])[CH3:3].[NH:34]1[CH2:39][CH2:38][O:37][CH2:36][CH2:35]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>C1COCC1.ClCCl>[CH2:2]([NH:4][C:5]([C:7]1[S:33][C:10]2[N:11]=[C:12]([NH2:32])[N:13]=[C:14]([C:15]3[CH:20]=[C:19]([O:21][CH2:22][CH2:23][N:34]4[CH2:39][CH2:38][O:37][CH2:36][CH2:35]4)[C:18]([Cl:30])=[CH:17][C:16]=3[Cl:31])[C:9]=2[CH:8]=1)=[O:6])[CH3:3]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8083MorpholineHCID 5049666Sodium triacetoxyborohydrideHCID 442209122-Amino-4-(2,4-dichloro-5-(2,2-diethoxyethoxy)-phenyl)-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl amide

생성물 1

HCID 59519252HCID 59519252, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

Hydrochloric acid was added to a solution of 2-Amino-4-(2,4-dichloro-5-(2,2-diethoxyethoxy)-phenyl)-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl amide in THF and the solution stirred for ˜18 hrs. Morpholine was added and the solution stirred, sodium triacetoxyborohydride was added and the resulting suspension stirred for ˜18 hrs. Dichloromethane was added and the mixture washed with aqueous ammonia (0.880), water and saturated aqueous sodium chloride solution. The solution was dried over anhydrous sodium sulphate and concentrated to a pale yellow solid. The crude product was purified by chromatography on silica eluting with mixtures of ethyl acetate and hexane.

후처리

  1. stirringthe solution stirred
  2. stirringthe resulting suspension stirred for ˜18 hrs
  3. washthe mixture washed with aqueous ammonia (0.880), water and saturated aqueous sodium chloride solution
  4. dry with materialThe solution was dried over anhydrous sodium sulphate
  5. concentrationconcentrated to a pale yellow solid
  6. customThe crude product was purified by chromatography on silica eluting with mixtures of ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-ceef8401fcdd42d4b4c441cc123e674c
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07820658B2

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