Phosphate → HCID 14645957、化合物

HRID 2249006ノート

反応式

HRID 2249006 の反応式
[F:1][C:2]1[C:10]([F:11])=[C:9]([F:12])[C:8]([F:13])=[C:7]([F:14])[C:3]=1[C@H:4]1[O:6][CH2:5]1.[Br-:15].[Li+].P([O-])([O-])([O-])=O>O1CCCC1.[Ni](Br)Br>[Br:15][CH2:5][C@@H:4]([C:3]1[C:2]([F:1])=[C:10]([F:11])[C:9]([F:12])=[C:8]([F:13])[C:7]=1[F:14])[OH:6]

参加物

6

反応物 3

HCID 1061PhosphateHCID 82050Lithium BromideHCID 11287268(2R)-2-(Pentafluorophenyl)oxirane

生成物 1

HCID 14645957HCID 14645957、化合物収率 70.1%

試薬・触媒・溶媒 2

HCID 278492Nickel(II) bromide触媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To an ice-cooled solution of 1.05 g of (R)-(+)-2,3,4,5,6-pentafluorostyrene oxide in 10 ml of tetrahydrofuran, was added dropwise a solution of Li2NiBr4, which was prepared by adding 2.19 g of nickel (II) bromide to a suspension of 1.74 g of lithium bromide in 20 ml of tetrahydrofuran. After completion of addition, the solution was stirred for 15 hours at room temperature. The resulted reaction mixture was poured into a 0.05 mol phosphate buffer, and was extracted with ether. The resultant extract was dried over magnesium sulfate, and the solvent was distilled off under reduced pressure, thereby obtaining 1.02 g of (R)-(-)-2-bromo-1-(pentafluorophenyl)ethanol containing 15% of (+)-2-bromo-2-(pentafluorophenyl)ethanol.

後処理

  1. customwas prepared
  2. additionAfter completion of addition
  3. customThe resulted reaction mixture
  4. extractionwas extracted with ether
  5. extractionThe resultant extract
  6. dry with materialwas dried over magnesium sulfate
  7. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-60c18f0946294ef48cf21ec118932877
出典データセット
uspto-grants-1991_08
特許番号
US05041641

反応ノート

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