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Aminoacetaldehyde dimethyl acetal → HCID 20093975, 화합물

HRID 273804
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HRID 273804 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[CH3:12])[N:5]=[C:4]([CH3:13])[N:3]=1.[CH3:14][O:15][CH:16]([O:19][CH3:20])[CH2:17][NH2:18]>O1CCCC1>[CH3:14][O:15][CH:16]([O:19][CH3:20])[CH2:17][NH:18][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[CH3:12])[N:5]=[C:4]([CH3:13])[N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 89728Aminoacetaldehyde dimethyl acetal2회HCID 200939884-Chloro-2,5-dimethylquinazoline

생성물 1

HCID 20093975HCID 20093975, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
5 °C

실험 절차

4. 14.15 g of crude 4-chloro-2,5-dimethylquinazoline are suspended in 300 ml of tetrahydrofuran, cooled to 5° C. and treated with 16.5 ml of 2,2-dimethoxyethylamine while stirring. The mixture is stirred at room temperature for 24 h., a further 10 ml of 2,2-dimethoxyethylamine are added thereto and the mixture is stirred for a further 40 h. The reaction mixture is evaporated in vacuum and the residue is partitioned between chloroform and saturated aqueous sodium hydrogen carbonate solution. The chloroform solution is evaporated in a vacuum. The residue (21 g) is chromatographed over 150 g of silica gel. 1.85 g of 4-(2,2-dimethoxyethylamino)-2,5-dimethylquinozoline are eluted with ethyl acetate. These are recrystallized from hexane. There are obtained 18.3 g of 4-(2,2-dimethoxyethyl-amino)-2,5-dimethylquinazoline of m.p. 48°-49° C.

후처리

  1. stirringThe mixture is stirred at room temperature for 24 h.
  2. stirringthe mixture is stirred for a further 40 h
  3. customThe reaction mixture is evaporated in vacuum
  4. customthe residue is partitioned between chloroform and saturated aqueous sodium hydrogen carbonate solution
  5. customThe chloroform solution is evaporated in a vacuum
  6. customThe residue (21 g) is chromatographed over 150 g of silica gel
  7. wash1.85 g of 4-(2,2-dimethoxyethylamino)-2,5-dimethylquinozoline are eluted with ethyl acetate
  8. customThese are recrystallized from hexane

출처 및 근거

ORD 기록
ord-3b6096abbc7c43bab331f6400489e532
출처 데이터셋
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05387585

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