Water → 2-(Benzyloxy)-5-iodobenzaldehyde

HRID 269593노트

반응식

HRID 269593 반응식
C(=O)([O-])[O-].[K+].[K+].[OH:7][C:8]1[CH:15]=[CH:14][C:13]([I:16])=[CH:12][C:9]=1[CH:10]=[O:11].[CH2:17](Cl)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.O>CN(C)C=O>[CH2:17]([O:7][C:8]1[CH:15]=[CH:14][C:13]([I:16])=[CH:12][C:9]=1[CH:10]=[O:11])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 2526125-Iodosalicylaldehyde

생성물 1

HCID 150434892-(Benzyloxy)-5-iodobenzaldehyde

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
120 °C

실험 절차

67.2 g (0.48 mol) of potassium carbonate are added to a solution of 100 g (0.40 mol) of 2-hydroxy-5-iodobenzaldehyde (Example 1A) in 1.5 l of dimethylformamide and, after a few minutes, 51 ml (0.44 mol) of benzyl chloride are added. The reaction mixture is stirred under reflux at 120° C. for 24 h. After stirring at RT for a further 24 h and the addition of 1.5 l of water, a solid crystallizes out. The precipitate is collected by suction filtration, washed twice with water and dried in vacuo. The solid is recrystallized from 230 ml of ethanol. 122.9 g (90% of theory) of product are obtained.

후처리

  1. stirringAfter stirring at RT for a further 24 h
  2. customa solid crystallizes out
  3. filtrationThe precipitate is collected by suction filtration
  4. washwashed twice with water
  5. customdried in vacuo
  6. customThe solid is recrystallized from 230 ml of ethanol
  7. custom122.9 g (90% of theory) of product are obtained

출처 및 근거

ORD 기록
ord-9e94ef8973c342148286ee8d143e61ba
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07446102B2

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