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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
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Hydrochloric Acid → Diisopropyl Ether

HRID 2263556
ノート
印刷プレビュー

反応式

HRID 2263556 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[Br:6][C:7]1[CH:12]=[CH:11][C:10]([C:13](=[O:15])[CH3:14])=[C:9]([OH:16])[CH:8]=1.C(N([CH2:22][CH3:23])CC)C.Cl>ClCCl>[C:13]([C:10]1[CH:11]=[CH:12][C:7]([Br:6])=[CH:8][C:9]=1[O:16][S:2]([CH3:1])(=[O:4])=[O:3])(=[O:15])[CH3:14].[CH:22]([O:15][CH:13]([CH3:10])[CH3:14])([CH3:23])[CH3:1]
参加物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 313Hydrochloric AcidHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 107274031-(4-Bromo-2-hydroxyphenyl)ethan-1-one

生成物 2

HCID 7914Diisopropyl EtherHCID 86071609Methanesulfonic acid 2-acetyl-5-bromophenyl ester

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

4.42 ml of methanesulphonyl chloride are added dropwise to a solution of 10.0 g 1-(4-bromo-2-hydroxy-phenyl)ethanone [30186-18-6] and 13.0 ml of triethylamine in 200 ml dichloromethane at 0° C. The reaction mixture is worked up after 1 hour by pouring into 250 ml cold 1N HCl and extracting with tert-butyl methyl ether (2×)—the combined organic layers are washed successively with water and brine, dried over sodium sulphate and concentrated by evaporation. The title compound is obtained as light yellow crystals from the residue by re-crystallization from diisopropyl ether. Rf=0.51 (1:1 EtOAc-heptane). Rt=3.94 (gradient I). m.p. 62.0-62.1° C.

後処理

  1. extractionextracting with tert-butyl methyl ether (2×)—the combined organic layers
  2. washare washed successively with water and brine
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-56149856062c48e1bb3e06601d07058f
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07851634B2

反応ノート

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