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Diethylamine → HCID 18924858, 화합물

HRID 1288823
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HRID 1288823 반응식
Cl[CH2:2][C:3]1[N:4]=[C:5]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[C:16]([O:22][CH3:23])[CH:15]=2)[C:6]2[C:11]([CH3:12])=[C:10]([CH3:13])[S:9][C:7]=2[N:8]=1.[CH2:24]([NH:26][CH2:27]C)C>ClCCl>[CH3:23][O:22][C:16]1[CH:15]=[C:14]([C:5]2[C:6]3[C:11]([CH3:12])=[C:10]([CH3:13])[S:9][C:7]=3[N:8]=[C:3]([CH2:2][N:26]([CH3:27])[CH3:24])[N:4]=2)[CH:19]=[CH:18][C:17]=1[O:20][CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8021DiethylamineHCID 18924851HCID 18924851, 화합물

생성물 1

HCID 18924858HCID 18924858, 화합물수율 44%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 2-chloromethyl-4-(3,4-dimethoxyphenyl)-5,6-dimethylthieno[2,3-d]pyrimidine (1.0 g), diethylamine (1.2 ml) and dichloromethane (30 ml) was stirred for 16 hours under reflux. The reaction mixture was concentrated under reduced pressure, which was dissolved in ethyl acetate. The ethyl acetate layer was washed with water and dried (MgSO4), then the solvent was distilled off. The residue was subjected to column chromatography on silica gel. From the fraction eluted with ethyl acetate-methanol (5:1, v/v), was obtained 4-(3,4-dimethoxyphenyl)-5,6-dimethyl-2-(N,N-dimethylamino-methyl)thieno[2,3-d]pyrimidine (0.49 g, 44%). Recrystallization from isopropyl ether gave colorless prisms, m.p.118°-120° C.

후처리

  1. temperatureunder reflux
  2. concentrationThe reaction mixture was concentrated under reduced pressure, which
  3. dissolutionwas dissolved in ethyl acetate
  4. washThe ethyl acetate layer was washed with water
  5. dry with materialdried (MgSO4)
  6. distillationthe solvent was distilled off
  7. washFrom the fraction eluted with ethyl acetate-methanol (5:1

출처 및 근거

ORD 기록
ord-dd322dead33a4bf28942748923428705
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05747486

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