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

HRID 973324ノート

反応式

HRID 973324 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 carton 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 carton are added to the residue
  6. filtrationthe solution is filtered
  7. customevaporated

出典と根拠

ORDレコード
ord-b7e036cfa088412792101cf37364bc61
出典データセット
uspto-grants-1977_10
特許番号
US04055595

反応ノート

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