Water → HCID 20137751, 화합물

HRID 1252873노트

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HRID 1252873 반응식
[S:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([S:11]([NH2:14])(=[O:13])=[O:12])[C:5]=2[S:4][CH2:3][CH2:2]1.C[Al](C)C.[CH3:19][O:20][C:21]1[CH:26]=[C:25]([CH3:27])[N:24]=[C:23]([NH:28][C:29](=O)[O:30]C)[N:22]=1.O>C(Cl)Cl.Cl.C(O)(=O)C>[CH3:19][O:20][C:21]1[CH:26]=[C:25]([CH3:27])[N:24]=[C:23]([NH:28][C:29]([NH:14][S:11]([C:10]2[C:5]3[S:4][CH2:3][CH2:2][S:1][C:6]=3[CH:7]=[CH:8][CH:9]=2)(=[O:12])=[O:13])=[O:30])[N:22]=1

참가 물질

8

반응물 4

HCID 962WaterHCID 13072161Methyl (4-methoxy-6-methylpyrimidin-2-yl)carbamateHCID 16682925TrimethylaluminumHCID 201377482,3-Dihydro-1,4-benzodithiine-5-sulfonamide

생성물 1

HCID 20137751HCID 20137751, 화합물

시약·촉매·용매 3

HCID 313Hydrochloric Acid촉매HCID 176Acetic Acid용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 2.5 g 1,4-benzodithian-5-sulfonamide, prepared in Example 18, in 50 ml methylene chloride at ambient temperature under nitrogen is added 5.5 ml trimethylaluminum (2M in toluene). After stirring 15 minutes at ambient temperature 2.0 g of methyl [4-methoxy-6-methylpyrimidin-2-yl]carbamate, prepared according to the procedure of Example 3, is added and the reaction mixture is heated at reflux for 16 hours. The reaction mixture is cooled to ambient temperature and 75 ml water, 10 ml glacial acetic acid, and 10 drops hydrochloric acid are sequentially added. The organic phase is separated, dried, and the solvent removed under reduced pressure to give an oil. Crystallization of the oil from n-butyl chloride/ether gives a solid.

후처리

  1. customprepared
  2. additionis added
  3. temperaturethe reaction mixture is heated
  4. temperatureat reflux for 16 hours
  5. customThe organic phase is separated
  6. customdried
  7. customthe solvent removed under reduced pressure
  8. customto give an oil
  9. customCrystallization of the oil from n-butyl chloride/ether
  10. customgives a solid

출처 및 근거

ORD 기록
ord-c61306c70b164cc3bc55b3a7885feef0
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04746358

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