ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Benzhydrol → Benzhydryl 4-bromo-3-oxobutyrate

HRID 1088656
ノート
印刷プレビュー

反応式

HRID 1088656 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 oof 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 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. customwere obtained

出典と根拠

ORDレコード
ord-986f486875834acb816ef69716e5b6cf
出典データセット
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04963542

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート