Dimethyl Sulfoxide → HCID 57785864, 화합물

HRID 1628707노트

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HRID 1628707 반응식
[Cl:1][C:2]1[C:10]2[N:9]=[C:8]3[N:11]([C:15]4[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:16]=4[C:22]([F:25])([F:24])[F:23])[CH2:12][CH2:13][CH2:14][N:7]3[C:6]=2[C:5]([CH2:26][OH:27])=[CH:4][CH:3]=1.C(N(CC)CC)C.CS(C)=O>ClCCl.C(=O)([O-])O.[Na+]>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH:26]=[O:27])=[C:6]2[C:10]=1[N:9]=[C:8]1[N:11]([C:15]3[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:16]=3[C:22]([F:24])([F:23])[F:25])[CH2:12][CH2:13][CH2:14][N:7]21

참가 물질

6

반응물 3

HCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 57785948HCID 57785948, 화합물

생성물 1

HCID 57785864HCID 57785864, 화합물수율 80%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 516892Sodium Bicarbonate용매

실험 절차

Sulfur trioxide-pyridine complex (23.4 g, 147 mmol) was added to a stirred solution of {9-chloro-1-[4-chloro-2-(trifluoromethyl)phenyl]-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-yl}methanol (8.72 g, 20.9 mmol), triethylamine (23.3 mL), and dimethyl sulfoxide (140 mL) in dichloromethane (30 mL) at room temperature, and the mixture was stirred at room temperature for 3 hr. The mixture was diluted with saturated aqueous sodium hydrogen carbonate, and extracted with ethyl acetate. The combined organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was washed with diisopropyl ether to give the title compound as a colorless powder (6.90 g, 16.7 mmol, 80%).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe combined organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. washThe residue was washed with diisopropyl ether

출처 및 근거

ORD 기록
ord-c325b497b77c4cc7bfea0ad89e553aa3
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785460B2

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