2,6-Difluorophenylacetic acid → 2-(2,6-Difluorophenyl)ethan-1-ol

HRID 471077

反応式

HRID 471077 の反応式
CSC.B.[F:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([F:12])[C:7]=1[CH2:13][C:14](O)=[O:15]>C1COCC1>[F:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([F:12])[C:7]=1[CH2:13][CH2:14][OH:15]

参加物

4

反応物 2

HCID 1235852,6-Difluorophenylacetic acidHCID 12423031(Dimethyl sulfide)trihydroboron

生成物 1

HCID 450906762-(2,6-Difluorophenyl)ethan-1-ol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of borane dimethyl sulfide complex (2M in THF, 26 mL) was added cautiously to a solution of 2-(2,6-difluorophenyl)acetic acid (3 g) in THF (50 mL) at 0° C. The reaction was then allowed to warm to RT and stirred for 3 h. The reaction was cooled in an ice bath and cautiously quenched with methanol (10 mL). The solvent was evaporated and the residue purified by silica gel chromatography eluting with 9:1 to 4:1 isohexane:ethyl acetate gradient. The fractions containing product were combined and evaporated to give the subtitled compound as a clear oil. Yield 2.2 g.

後処理

  1. temperatureThe reaction was cooled in an ice bath
  2. customcautiously quenched with methanol (10 mL)
  3. customThe solvent was evaporated
  4. customthe residue purified by silica gel chromatography
  5. washeluting with 9:1 to 4:1 isohexane
  6. additionThe fractions containing product
  7. customevaporated

出典と根拠

ORDレコード
ord-eb2c5d41310645ca8883a1856a04ea2f
出典データセット
uspto-grants-2014_01
特許番号
US08629271B2

関連ノート

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