4-Chlororesorcinol → HCID 13246701、化合物

HRID 2412304ノート

反応式

HRID 2412304 の反応式
[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([OH:6])=[CH:4][C:3]=1[OH:9].[Cl:10][C:11]1([Cl:16])[CH2:13][CH:12]1[CH2:14]Br.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN(C)C=O>[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([OH:6])=[CH:4][C:3]=1[O:9][CH2:14][CH:12]1[CH2:13][C:11]1([Cl:16])[Cl:10].[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([O:6][CH2:14][CH:12]2[CH2:13][C:11]2([Cl:16])[Cl:10])=[CH:4][C:3]=1[OH:9]

参加物

7

反応物 4

HCID 17314-ChlororesorcinolHCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 47395822-(Bromomethyl)-1,1-dichlorocyclopropane

生成物 2

HCID 13246701HCID 13246701、化合物HCID 13368146HCID 13368146、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

In 700 ml of N,N-dimethylformamide, there was dissolved 181 g of 4-chlororesorcinol. To the solution, there were added 283 g of (2,2-dichlorocyclopropyl)methyl bromide, 207 g of anhydrous potassium carbonate and 4 g of sodium iodide. The mixture was stirred at 90° C. for 15 hours, then poured into ice water and extracted with diethyl ether. The ether layer was washed with water and dried over anhydrous magnesium sulfate, and the solvent was then distilled off. The oily residue was subjected to preparatory high-speed liquid chromatography to give 93 g of 4-chloro-3-[(2,2-dichlorocyclopropyl)methoxy]phenol and 5 g of 2-chloro-5-[(2,2-dichlorocyclopropyl)methoxy]phenol.

後処理

  1. extractionextracted with diethyl ether
  2. washThe ether layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was then distilled off

出典と根拠

ORDレコード
ord-48ea252fc729446b89f5c716e9ac2a6a
出典データセット
uspto-grants-1985_01
特許番号
US04491465

反応ノート

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