Potassium Iodide → N-[4-bromo-3-(1-methyl-2-oxopropoxy)phenyl]-3,4,5,6-tetrahydrophthalimide

HRID 904781

反応式

HRID 904781 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11]3[CH2:14][CH2:15][CH2:16][CH2:17][C:10]=3[C:9]2=[O:18])=[CH:4][C:3]=1[OH:19].Cl[CH:21]([CH3:25])[C:22](=[O:24])[CH3:23].C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CC(C)=O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:9](=[O:18])[C:10]3[CH2:17][CH2:16][CH2:15][CH2:14][C:11]=3[C:12]2=[O:13])=[CH:4][C:3]=1[O:19][CH:21]([CH3:25])[C:22](=[O:24])[CH3:23]

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 200263-Chloro-2-butanoneHCID 12769237N-(4-bromo-3-hydroxyphenyl)-3,4,5,6-tetrahydrophthalimide

生成物 1

HCID 13290479N-[4-bromo-3-(1-methyl-2-oxopropoxy)phenyl]-3,4,5,6-tetrahydrophthalimide

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 4.0 g. of N-(4-bromo-3-hydroxyphenyl)-3,4,5,6-tetrahydrophthalimide, 2.0 g. of 3-chloro-2-butanone, 2.1 g. of potassium carbonate, 1.0 g. of potassium iodide and 30 ml. of acetone was refluxed with stirring for 3 hours. The precipitate was separated by a filtration and the filtrate was concentrated under a reduced pressure and the residue was purified by a chromatography on a column of silica gel (developing solvent: ethyl acetate:n-hexane of 2:3) to obtain 4.2 g. of Compound No. 24 shown in Table 1.

後処理

  1. additionA mixture of 4.0 g
  2. customThe precipitate was separated by a filtration
  3. concentrationthe filtrate was concentrated under a reduced pressure
  4. customthe residue was purified by a chromatography on a column of silica gel (developing solvent: ethyl acetate:n-hexane of 2:3)
  5. customto obtain 4.2 g

出典と根拠

ORDレコード
ord-7722eb1ec1544be9a38cb0e2057a7fde
出典データセット
uspto-grants-1983_12
特許番号
US04420327

関連ノート

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