Triethylamine → HCID 21710564, 화합물

HRID 651043노트

반응식

HRID 651043 반응식
[CH2:1]([C:8]([OH:15])([CH2:11][CH2:12][CH2:13][CH3:14])[CH2:9][OH:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH3:23][S:24](Cl)(=[O:26])=[O:25]>ClCCl.C(OCC)(=O)C>[CH3:23][S:24]([CH:9]([OH:10])[C:8]([CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)([OH:15])[CH2:11][CH2:12][CH2:13][CH3:14])(=[O:26])=[O:25]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 21710574HCID 21710574, 화합물

생성물 1

HCID 21710564HCID 21710564, 화합물수율 96.4%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

To a stirred solution of the product from Example 19B (416 mg, 2.0 mmol) in 4 mL of dichloromethane at 0° C. was added triethylamine (0.34 mL, 2.4 mmol) followed by the addition of methanesulfonyl chloride (0.17 mL, 2.2 mmol). The mixture was placed in a refrigerator overnight. The resulting cloudy mixture was diluted with ethyl acetate and extracted with water, 3N aqueous HCl, water and brine, dried (Na2SO4), filtered, and concentrated to provide 552 mg (96%) of the title compound as an oil that was used directly.

후처리

  1. customwas placed in a refrigerator overnight
  2. extractionextracted with water, 3N aqueous HCl, water and brine
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8f43f48aa0d04adcad70825f38e06395
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06277871B1

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