Phosphate → HCID 14645957, 화합물

HRID 2249006노트

반응식

HRID 2249006 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 14645957HCID 14645957, 화합물수율 70.1%

시약·촉매·용매 2

HCID 278492Nickel(II) bromide촉매HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-60c18f0946294ef48cf21ec118932877
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05041641

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