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Dimethyl Sulfoxide → HCID 10104772, 화합물

HRID 538681
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HRID 538681 반응식
CS(C)=O.C(Cl)(C(Cl)=O)=O.[CH2:11]([N:18]1[CH2:23][CH2:22][CH2:21][CH2:20][CH:19]1[CH2:24][CH2:25][OH:26])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>C(Cl)Cl>[CH2:11]([N:18]1[CH2:23][CH2:22][CH2:21][CH2:20][CH:19]1[CH2:24][CH:25]=[O:26])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 679Dimethyl SulfoxideHCID 65578Oxalyl chlorideHCID 102425512-(1-Benzylpiperidin-2-yl)ethan-1-ol

생성물 1

HCID 10104772HCID 10104772, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

To a stirred solution of DMSO (5.84 mL, 82.2 mmol) in dry DCM (220 mL) was added (COCl)2 (3.55 mL, 41.1 mmol) at −78° C. and the mixture stirred at same temperature for 20 minutes. A solution of compound 49 (6 g, 27.4 mmol) in DCM (30 mL) was then added slowly and the reaction mixture was stirred at −78° C. for 1 hour. TEA (13.8 mL, 137 mmol) was added at −78° C. and the reaction mixture was stirred and allowed to come to rt. The reaction mixture was diluted with DCM and the organic layer was washed with water and brine, dried over anhydrous Na2SO4, filtered and concentrated to provide sticky compound 50.

후처리

  1. stirringthe reaction mixture was stirred at −78° C. for 1 hour
  2. stirringthe reaction mixture was stirred
  3. customto come to rt
  4. washthe organic layer was washed with water and brine
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-915e4ff0ff5e4bcb83f002c4e5a28fcc
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08865741B2

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