Triethylamine → Methyl 2-chloro-2-(2-fluoro-4,5-dimethoxyphenyl)acetate

HRID 1438181노트

반응식

HRID 1438181 반응식
[F:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([O:10][CH3:11])=[CH:4][C:3]=1[CH:12](O)[C:13]([O:15][CH3:16])=[O:14].C(N(CC)CC)C.S([Cl:29])(C)(=O)=O>C(Cl)Cl>[Cl:29][CH:12]([C:3]1[CH:4]=[C:5]([O:10][CH3:11])[C:6]([O:8][CH3:9])=[CH:7][C:2]=1[F:1])[C:13]([O:15][CH3:16])=[O:14]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 57448188Methyl 2-(2-fluoro-4,5-dimethoxyphenyl)-2-hydroxyacetate

생성물 1

HCID 57448189Methyl 2-chloro-2-(2-fluoro-4,5-dimethoxyphenyl)acetate수율 89%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To 139A (280 mg, 1.2 mmol) in CH2Cl2 (5 mL) at 0° C. was added triethylamine (0.42 mL, 3.0 mmol) followed by mesyl chloride (0.12 mL, 1.5 mmol). After stirring at rt overnight, the reaction was filtered, concentrated and purified via silica gel chromatography (0-30% ethyl acetate/hexanes) to provide 139B (268 mg, 89%).

후처리

  1. filtrationthe reaction was filtered
  2. concentrationconcentrated
  3. custompurified via silica gel chromatography (0-30% ethyl acetate/hexanes)

출처 및 근거

ORD 기록
ord-3da6bb0fa6c04fc6bfa2205279827696
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07622585B2

반응 노트

불러오는 중…