Diethyl Ether → 2,3,6-Trifluorobenzyl alcohol

HRID 1638678

反応式

HRID 1638678 の反応式
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]

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 6356Boron trifluorideHCID 5200622,3,6-Trifluorobenzoic acidHCID 178418435HCID 178418435、化合物

生成物 1

HCID 1455002,3,6-Trifluorobenzyl alcohol収率 102%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a7ed83656f0941eaaade34c9a5206a37
出典データセット
uspto-grants-1989_11
特許番号
US04880806

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