1-Chloro-1,1,3,3,3-pentafluoro-2-propanone → 1,1,1,3,3-Pentafluoro-2-(4-ethoxyphenyl)-3-chloropropan-2-ol

HRID 483727

反応式

HRID 483727 の反応式
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)[CH3:2].[Cl:10][C:11]([F:19])([F:18])[C:12]([C:14]([F:17])([F:16])[F:15])=[O:13].[Cl-].[Al+3].[Cl-].[Cl-]>C(Cl)(Cl)Cl>[F:15][C:14]([F:17])([F:16])[C:12]([C:7]1[CH:8]=[CH:9][C:4]([O:3][CH2:1][CH3:2])=[CH:5][CH:6]=1)([OH:13])[C:11]([F:19])([F:18])[Cl:10]

参加物

5

反応物 3

HCID 66011-Chloro-1,1,3,3,3-pentafluoro-2-propanoneHCID 7674PhenetoleHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 138807621,1,1,3,3-Pentafluoro-2-(4-ethoxyphenyl)-3-chloropropan-2-ol

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
120 °C

実験手順

A mixture of ethoxybenzene (67 g), chloropentafluoroacetone (100 g) and aluminium chloride (7 g) was charged to a Hastalloy lined cell at -78° C, the cell sealed and heated to 120° C for 8 hours. After cooling and venting, the residue was taken up in chloroform and filtered through silica gel. After removal of the solvent by evaporation the residual solid was recrystallised from n-hexane to yield several crops of 1,1,1,3,3-pentafluoro-2-(4-ethoxyphenyl)-3-chloropropan-2-ol. (Total 70 g) mp. 84°-86° C.

後処理

  1. additionwas charged to a Hastalloy
  2. customat -78° C
  3. customthe cell sealed
  4. temperatureAfter cooling
  5. filtrationfiltered through silica gel
  6. customAfter removal of the solvent
  7. customby evaporation the residual solid
  8. customwas recrystallised from n-hexane

出典と根拠

ORDレコード
ord-dcdfcf8fab2f45d09b224096d3eb9f89
出典データセット
uspto-grants-1993_07
特許番号
US05225607

関連ノート

読み込み中…