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Benzhydrol → Benzhydryl 4-bromo-3-oxobutyrate

HRID 444557
ノート
印刷プレビュー

反応式

HRID 444557 の反応式
C=C1OC(=O)C1.BrBr.[CH:9]([OH:22])([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[Br:23][CH2:24][C:25](=[O:30])[CH2:26][C:27](Br)=[O:28]>C(Cl)Cl.C(N(CC)CC)C>[Br:23][CH2:24][C:25](=[O:30])[CH2:26][C:27]([O:22][CH:9]([C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[O:28]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 7037BenzhydrolHCID 12661DiketeneHCID 24408BromineHCID 128310484-Bromo-3-oxobutanoyl bromide

生成物 1

HCID 15080911Benzhydryl 4-bromo-3-oxobutyrate

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒3 回
HCID 8471
Triethylamine
溶媒

反応条件

温度
0 °C

実験手順

In 10.5 ml of methylene chloride there were dissolved 2.1 g of diketene, and at a temperature not exceeding -30° C., a solution of 4.0 g of bromine in 12.5 ml of methylene chloride was added dropwise to the solution with stirring. After the dropwise addition was completed, the mixture was maintained at 0° C. for 10 minutes. Separately, 3.68 g of benzhydrol were dissolved in 25 ml of methylene chloride, followed by addition of 2.02 g of triethylamine. Under stirring at a temperature not exceeding -30° C., the solution of bromoacetoacetyl bromide prepared above was added dropwise. After the dropwise addition, the mixture was stirred at 0° C. for 40 minutes, at the end of which time it was washed with water. After drying over magnesium sulfate the solvent was distilled off under reduced pressure, whereupon 6.99 g of benzhydryl 4-bromo-3-oxobutyrate there were obtained.

後処理

  1. customexceeding -30° C.
  2. additionAfter the dropwise addition
  3. stirringUnder stirring at a temperature not
  4. customexceeding -30° C.
  5. additionabove was added dropwise
  6. additionAfter the dropwise addition
  7. stirringthe mixture was stirred at 0° C. for 40 minutes, at the end of which time it
  8. washwas washed with water
  9. dry with materialAfter drying over magnesium sulfate the solvent
  10. distillationwas distilled off under reduced pressure, whereupon 6.99 g of benzhydryl 4-bromo-3-oxobutyrate
  11. customthere were obtained

出典と根拠

ORDレコード
ord-6588f45014f0496398f74ee17145e6d1
出典データセット
uspto-grants-1981_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04264595

反応ノート

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