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Triethylamine → HCID 57988792, 화합물

HRID 889034
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HRID 889034 반응식
[OH:1][CH2:2][CH:3]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:9]=2)[C:4]1=[O:18].C(N(CC)CC)C.[CH3:26][S:27](Cl)(=[O:29])=[O:28].C([O-])(O)=O.[Na+]>ClCCl>[O:18]=[C:4]1[CH:3]([CH2:2][O:1][S:27]([CH3:26])(=[O:29])=[O:28])[CH2:7][CH2:6][N:5]1[C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:15])([F:16])[F:17])[CH:9]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 516892Sodium BicarbonateHCID 19434450HCID 19434450, 화합물

생성물 1

HCID 57988792HCID 57988792, 화합물수율 113.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

A mixture of 3-hydroxymethyl-1-(3-trifluoromethyl-phenyl)-pyrrolidin-2-one obtained in step 3 (0.17 g, 0.6 mmol), dichloromethane (8 ml) and triethyl amine (0.085 g, 0.84 mol) was cooled to 0° C. and stirred for 15 min at that temperature. Methane sulfonyl chloride (0.090 g, 0.78 mmol) was added to the mixture over a period of 5 min and the reaction mixture was stirred for 1.5 hrs at 10-15° C. To this reaction mixture saturated NaHCO3 solution (10 ml) was added and the organic layer was separated. The aqueous layer was extracted with dichloromethane. The combined organic layer was washed with saturated brine solution, dried over Na2SO4 and evaporated to obtain methanesulfonic acid 2-oxo-1-(3-trifluoromethyl-phenyl)-pyrrolidin-3-ylmethyl ester as a brown oil (0.23 g, 100%).

후처리

  1. stirringthe reaction mixture was stirred for 1.5 hrs at 10-15° C
  2. customthe organic layer was separated
  3. extractionThe aqueous layer was extracted with dichloromethane
  4. washThe combined organic layer was washed with saturated brine solution
  5. dry with materialdried over Na2SO4
  6. customevaporated

출처 및 근거

ORD 기록
ord-e2a96215764243dbb3d236f7f7ae3eab
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08252797B2

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