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Water → HCID 57772620, 화합물

HRID 1522722
노트
인쇄 미리보기

반응식

HRID 1522722 반응식
[OH-].[K+].[Br:3][C:4]1[CH:9]=[CH:8][C:7]([CH2:10][C:11]([CH2:13][C:14]2[CH:19]=[CH:18][C:17]([Br:20])=[CH:16][CH:15]=2)=[O:12])=[CH:6][CH:5]=1.[Br:21][C:22]1[CH:27]=[CH:26][C:25]([C:28]([C:30]([C:32]2[CH:37]=[CH:36][C:35]([Br:38])=[CH:34][CH:33]=2)=O)=O)=[CH:24][CH:23]=1.O>C(O)C.ClCCl>[Br:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[C:11](=[O:12])[C:13]([C:14]3[CH:15]=[CH:16][C:17]([Br:20])=[CH:18][CH:19]=3)=[C:28]([C:25]3[CH:26]=[CH:27][C:22]([Br:21])=[CH:23][CH:24]=3)[C:30]=2[C:32]2[CH:33]=[CH:34][C:35]([Br:38])=[CH:36][CH:37]=2)=[CH:6][CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 14797Potassium HydroxideHCID 964304,4'-DibromobenzilHCID 12420215Bis(4-bromobenzyl) ketone

생성물 1

HCID 57772620HCID 57772620, 화합물수율 68%

시약·촉매·용매 2

HCID 702Ethanol용매2회
HCID 6344
Dichloromethane
용매

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온도
70 °C

실험 절차

A solution of potassium hydroxide (230 mg, 4.1 mmol) in ethanol (5 cm3) was added to a solution of (13) (3.01 g, 8.2 mmol) and 4,4′-dibromobenzil (3.01 g, 8.2 mmol) in ethanol (45 cm3) at 70° C., and the reaction was stirred at 70° C. for 4 hours. Water (200 cm3) and dichloromethane (200 cm3) were added, and the layers were separated. The organic layer was washed with brine (200 cm3) and dried over magnesium sulfate. The solvent was removed to leave a dark purple solid. The crude product was passed through a plug of silica, and then recrystallised from a dichloromethane/ethanol mixture to give (14) as a dark purple crystalline solid (3.87 g, 68%).

후처리

  1. customthe layers were separated
  2. washThe organic layer was washed with brine (200 cm3)
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was removed
  5. customto leave a dark purple solid
  6. customrecrystallised from a dichloromethane/ethanol mixture

출처 및 근거

ORD 기록
ord-e6bd9eb56a2e41f696ed845ac40c4406
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09078330B2

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