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4-Methoxy-6-methylpyrimidin-2-amine → HCID 178468247, 화합물

HRID 1249256
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HRID 1249256 반응식
[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([CH3:10])[N:3]=1.[CH2:11]([O:13][C:14](=[N:18][S:19]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[O:28][CH:29]([F:31])[F:30])(=[O:21])=[O:20])OCC)[CH3:12]>O1CCCC1.CCOCC>[F:31][CH:29]([F:30])[O:28][C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=1[S:19]([NH:18][C:14](=[N:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([CH3:10])[N:3]=1)[O:13][CH2:11][CH3:12])(=[O:21])=[O:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 5872364-Methoxy-6-methylpyrimidin-2-amineHCID 54050282N-(2-difluoromethoxybenzenesulfonyl)-imidocarbonic acid diethyl ester

생성물 1

HCID 178468247HCID 178468247, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 11.2 g (0.1 mol) of potassium tertbutylate in 125 ml of tetrahydrofuran are added at room temperature, with stirring, 13.9 g (0.1 mol) of 2-amino-4-methoxy-6-methylpyrimidine. Stirring is maintained for 2 hours at room temperature, and 32.3 g (0.1 mol) of N-(2-difluoromethoxy-benzenesulfonyl)-imido carbonic acid diethyl ester (obtained according to Example 1) are then added, the reaction mixture being stirred for a further 20 hours. The mixture is subsequently concentrated by evaporation, and the residue is taken up in water and rendered acid with hydrochloric acid. The acid solution is extracted with ethyl acetate; the organic phases are then collected, dried, and concentrated by evaporation to leave a solid residue, which is suspended in ether and again filtered off. The yield is 34.5 g (83% of theory) of the above sulfonylisourea, m.p. 131°-133° C.

후처리

  1. stirringStirring
  2. stirringthe reaction mixture being stirred for a further 20 hours
  3. concentrationThe mixture is subsequently concentrated by evaporation
  4. extractionThe acid solution is extracted with ethyl acetate
  5. customthe organic phases are then collected
  6. customdried
  7. concentrationconcentrated by evaporation
  8. customto leave a solid residue, which
  9. filtrationagain filtered off

출처 및 근거

ORD 기록
ord-f781ecb9871e4894a0c7b09d6e4887d3
출처 데이터셋
uspto-grants-1986_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04629802

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