4-Chlororesorcinol → HCID 13246701, 화합물

HRID 2412304노트

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HRID 2412304 반응식
[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]

참가 물질

7

반응물 4

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

생성물 2

HCID 13246701HCID 13246701, 화합물HCID 13368146HCID 13368146, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-48ea252fc729446b89f5c716e9ac2a6a
출처 데이터셋
uspto-grants-1985_01
특허 번호
US04491465

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