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

HRID 2419926ノート

反応式

HRID 2419926 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-abaf7e36b7ca4629afed72d296687c08
出典データセット
uspto-grants-1978_08
特許番号
US04107329

反応ノート

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