Diethyl Ether → 2,3,6-Trifluorobenzyl alcohol

HRID 1638678

반응식

HRID 1638678 반응식
B.[Na].[F:3][C:4]1[CH:12]=[CH:11][C:10]([F:13])=[C:9]([F:14])[C:5]=1[C:6](O)=[O:7].B(F)(F)F.CCOCC>O1CCCC1>[F:14][C:9]1[C:10]([F:13])=[CH:11][CH:12]=[C:4]([F:3])[C:5]=1[CH2:6][OH:7]

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 6356Boron trifluorideHCID 5200622,3,6-Trifluorobenzoic acidHCID 178418435HCID 178418435, 화합물

생성물 1

HCID 1455002,3,6-Trifluorobenzyl alcohol수율 102%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

To a solution of sodium boron hydride (51.6 g) in tetrahydrofuran (500 ml) is added dropwise a solution of 2,5,6-trifluorobenzoic acid (120 g) in tetrahydrofuran (200 ml) with stirring at below 10° C., and thereto is further added dropwise a solution of BF3.(C2H5)2O (232 ml) in tetrahydrofuran (500 ml) under ice cooling. The mixture is stirred at room temperature overnight. The reaction mixture is poured into ice water (1.5 liter) and is extracted with diethyl ether. The extract is dried over magnesium sulfate and the solvent is distilled off under reduced pressure to give 2,3,6-trifluorobenzyl alcohol (112.7 g), as pale yellow oil, b.p. 112° C. (30 mmHg).

후처리

  1. stirringThe mixture is stirred at room temperature overnight
  2. extractionis extracted with diethyl ether
  3. dry with materialThe extract is dried over magnesium sulfate
  4. distillationthe solvent is distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-a7ed83656f0941eaaade34c9a5206a37
출처 데이터셋
uspto-grants-1989_11
특허 번호
US04880806

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