Hydrochloric Acid → HCID 9944111、化合物

HRID 1797401ノート

反応式

HRID 1797401 の反応式
[BH4-].[Na+].[CH3:3][C:4]([O:15][C:16]1[CH:21]=[C:20]([CH3:22])[CH:19]=[C:18]([CH3:23])[C:17]=1[CH3:24])([CH3:14])[C:5]([C:7]1[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][CH:8]=1)=[O:6].Cl>[OH-].[Na+].CO>[CH3:14][C:4]([O:15][C:16]1[CH:21]=[C:20]([CH3:22])[CH:19]=[C:18]([CH3:23])[C:17]=1[CH3:24])([CH3:3])[CH:5]([C:7]1[CH:8]=[CH:9][C:10]([CH3:13])=[CH:11][CH:12]=1)[OH:6]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 9879261HCID 9879261、化合物

生成物 1

HCID 9944111HCID 9944111、化合物収率 100%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 14798Sodium Hydroxide溶媒

反応条件

温度
35 °C

実験手順

A solution of sodium borohydride (25.7 g) in 0.1N NaOH (202 mL) was added dropwise to a suspension of 2-methyl-1-(4-methylphenyl)-2-(2,3,5-trimethylphenoxy)-1-propanone (251.9 g) in methanol (2519 mL). The mixture was stirred at 35° C. for 3 hours. After the mixture was adjusted to pH 7 by addition of 1N HCl under ice-cooling, methanol was distilled off, followed by extraction with toluene (2015 mL). The extract was washed with water, and the solvent was distilled off to quantitatively obtain the title compound as an oil (253.7 g).

後処理

  1. temperaturecooling
  2. distillationmethanol was distilled off
  3. extractionfollowed by extraction with toluene (2015 mL)
  4. washThe extract was washed with water
  5. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-5a51473270354f18875136bc0acf72e4
出典データセット
uspto-grants-2006_04
特許番号
US07034166B2

反応ノート

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