Dimethylformamide → (+/-)-2-(2-Naphthylmethoxy)-3,3,3-trifluoro-2-methylpropionyl chloride

HRID 2419926노트

반응식

HRID 2419926 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH2:11][O:12][C:13]([CH3:21])([C:17]([F:20])([F:19])[F:18])[C:14](O)=[O:15].S(Cl)([Cl:24])=O.CN(C)C=O>C1C=CC=CC=1>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH2:11][O:12][C:13]([CH3:21])([C:17]([F:20])([F:19])[F:18])[C:14]([Cl:24])=[O:15]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 13384287(+/-)-2-(2-Naphthylmethoxy)-3,3,3-trifluoro-2-methylpropionic acid

생성물 1

HCID 20314457(+/-)-2-(2-Naphthylmethoxy)-3,3,3-trifluoro-2-methylpropionyl chloride

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A solution of (±)-2-(2-naphthylmethoxy)-3,3,3-trifluoro-2-methylpropionic acid (6.0 g.), thionyl chloride (7.5 ml.) and dimethylformamide (0.2 g.) in benzene (50 ml.) is heated under reflux for 10 minutes. The mixture is evaporated, benzene (20 ml.) is added and the evaporation repeated twice. Light petroleum (b.p. 40°-60° C., 150 ml.) and carbon are added to the residue, and the solution is filtered and evaporated to give (±)-2-(2-naphthylmethoxy)- 3,3,3-trifluoro-2-methylpropionyl chloride (5.35 g.) m.p, 39°-43° C.

후처리

  1. temperatureunder reflux for 10 minutes
  2. customThe mixture is evaporated
  3. additionbenzene (20 ml.) is added
  4. customthe evaporation
  5. additionLight petroleum (b.p. 40°-60° C., 150 ml.) and carbon are added to the residue
  6. filtrationthe solution is filtered
  7. customevaporated

출처 및 근거

ORD 기록
ord-abaf7e36b7ca4629afed72d296687c08
출처 데이터셋
uspto-grants-1978_08
특허 번호
US04107329

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