Hexafluoropropylene → HCID 131729307、化合物

HRID 656717ノート

反応式

HRID 656717 の反応式
FCC(F)(F)C(F)(F)O.[C:10]([CH:17]([O:19][CH2:20][C:21]([C:24]([F:27])([F:26])[F:25])([F:23])[F:22])[OH:18])([C:13]([F:16])([F:15])[F:14])([F:12])[F:11].C(=O)([O-])[O-].[K+].[K+].[F:34][C:35]([F:42])([F:41])[C:36]([F:40])=[C:37]([F:39])[F:38].C(C(COC(C(C(F)(F)F)F)(F)F)(F)F)(F)(F)F>O.C(#N)C>[C:10]([CH:17]([O:18][C:37]([CH:36]([C:35]([F:42])([F:41])[F:34])[F:40])([F:39])[F:38])[O:19][CH2:20][C:21]([C:24]([F:25])([F:26])[F:27])([F:22])[F:23])([C:13]([F:16])([F:15])[F:14])([F:12])[F:11]

参加物

8

反応物 5

HCID 8302HexafluoropropyleneHCID 11430Potassium CarbonateHCID 16878528302-70-72 回HCID 27785191H,1H,2'H-Perfluorodipropyl etherHCID 713784112,2,3,3,3-Pentafluoro-1-(2,2,3,3,3-pentafluoropropoxy)propan-1-ol

生成物 1

HCID 131729307HCID 131729307、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
40 °C

実験手順

The entire contents of the pentafluoropropanol solution (containing the desired C2F5CH(OH)OCH2C2F5) were placed in a 600 mL Parr reaction vessel along with acetonitrile (167 g) and powdered potassium carbonate (2.9 g). The reactor was sealed, evacuated and heated to 40° C. Hexafluoropropene (64.8 g, 0.43 mole) was added in portions over about two hours and the reactor then held at temperature overnight. The reaction mixture was worked up by pouring into water and washing the resulting lower phase three times with water followed by distillation. The distillation afford a main fraction of boiling point 142° C. The product identity was confirmed by GC-MS and H-1 and F-19 NMR as a mixture of diastereomers in a ratio of 55/45%. One diastereomeric fraction was thought to contain SS and RR enantiomers and the other SR and RS enantiomers. The NMR data showed that the product contained about 4.2% olefin [—OCF═CFCF3] as a 43/57% cis/trans mixture. The excess pentafluoropropanol was converted to CF3CF2CH2OCF2CFHCF3 which was removed during the distillation.

後処理

  1. customThe reactor was sealed
  2. customevacuated
  3. customthen held at temperature overnight
  4. washwashing the resulting lower phase three times with water
  5. distillationfollowed by distillation
  6. distillationThe distillation
  7. customafford a main fraction of boiling point 142° C
  8. customwas removed during the distillation

出典と根拠

ORDレコード
ord-c6270098ba2b4cc7bed52f03596adf3c
出典データセット
uspto-grants-2011_12
特許番号
US08071816B2

反応ノート

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