Water → 1,3-Bis(p-carbobenzyloxyphenoxymethyl)-benzene

HRID 329996

반응식

HRID 329996 반응식
[CH2:1]([O:8][C:9](=[O:17])[C:10]1[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:18](=[O:21])([O-])[O-:19].[Na+].[Na+].[C:24]1([CH2:32]Cl)[CH:29]=[CH:28][CH:27]=[C:26]([CH2:30]Cl)[CH:25]=1.[OH2:34]>CN(C)C=O>[C:9]([C:10]1[CH:11]=[CH:12][C:13]([O:16][CH2:32][C:24]2[CH:29]=[CH:28][CH:27]=[C:26]([CH2:30][O:34][C:13]3[CH:12]=[CH:11][C:10]([C:18]([O:19][CH2:1][C:2]4[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=4)=[O:21])=[CH:15][CH:14]=3)[CH:25]=2)=[CH:14][CH:15]=1)([O:8][CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)=[O:17]

참가 물질

6

반응물 4

HCID 962WaterHCID 7180Benzyl 4-HydroxybenzoateHCID 10340Sodium CarbonateHCID 12275Benzene, 1,3-bis(chloromethyl)-

생성물 1

HCID 143236701,3-Bis(p-carbobenzyloxyphenoxymethyl)-benzene수율 26.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To a solution of p-hydroxybenzoic acid benzyl ester (45.6 g, 0.2 mol) in 200 ml N,N-dimethylformamide, sodium carbonate (10.6 g, 0.1 mol) was added and stirred for 10 minutes at room temperature. Then a solution of m-xylylenedichloride (17.3 g, 0.1 mol) in 100 ml of N,N-dimethylformamide was added in drops to the reaction mixture in 10 minutes. The reaction mixture stirred at 113° C. for 4 hours, cooled and blown into water, and the obtained precipitate was filtered, rinsed with water. Then crued product was suspended in methanol and stirred at 60° C. for 30 minutes, cooled, filtered, and gave 15.8 g (yield 26.9%) of 1,3-bis(p-carbobenzyloxyphenoxymethyl)-benzene: m.p. 92.5°-93.8° C.

후처리

  1. stirringThe reaction mixture stirred at 113° C. for 4 hours
  2. temperaturecooled
  3. filtrationthe obtained precipitate was filtered
  4. washrinsed with water
  5. stirringstirred at 60° C. for 30 minutes
  6. temperaturecooled
  7. filtrationfiltered

출처 및 근거

ORD 기록
ord-1c78c21147d74db4ad612f4064d9a100
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04894359

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