Dimethylformamide → 1,4-Bis(p-carbobenzyloxyphenoxymethyl)benzene

HRID 329997

反応式

HRID 329997 の反応式
[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.CN(C)[CH:20]=[O:21].[C:23]1([CH2:31]Cl)[CH:28]=[CH:27][C:26]([CH2:29]Cl)=[CH:25][CH:24]=1>O>[C:9]([C:10]1[CH:11]=[CH:12][C:13]([O:16][CH2:31][C:23]2[CH:28]=[CH:27][C:26]([CH2:29][O:16][C:13]3[CH:12]=[CH:11][C:10]([C:9]([O:21][CH2:20][C:3]4[CH:2]=[CH:7][CH:6]=[CH:5][CH:4]=4)=[O:8])=[CH:15][CH:14]=3)=[CH:25][CH:24]=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]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 7180Benzyl 4-HydroxybenzoateHCID 12171alpha,alpha'-Dichloro-p-xylene

生成物 1

HCID 143236711,4-Bis(p-carbobenzyloxyphenoxymethyl)benzene収率 33.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

To a solution of p-hydroxybenzoic acid benzyl ester (68.4 g, 0.3 mol) in N,N-dimethylformamide (274 g) sodium carbonate (15.9 g, 0.15 mol) was added, and stirred at 100° C. Then, p-xylylenedichloride (26.2 g, 0.15 mol) was added to the reaction mixture in 10 minutes, and stirred at 100° C. for one hour. Water was added to the resultant to separate a clued precipitate. The precipitate was filtered, added to N,N-dimethylformamide to be dissolved at 90° C., cooled, filtered, and dried to give a white crystal of 1,4-bis(p-carbobenzyloxyphenoxymethyl)benzene (27.8 g, yield 33.0): m.p. 154°-157° C.

後処理

  1. stirringstirred at 100° C. for one hour
  2. customto separate a clued precipitate
  3. filtrationThe precipitate was filtered
  4. additionadded to N,N-dimethylformamide
  5. dissolutionto be dissolved at 90° C.
  6. temperaturecooled
  7. filtrationfiltered
  8. customdried

出典と根拠

ORDレコード
ord-5d57cfe81a4249d7acd7f41e61b5abc6
出典データセット
uspto-grants-1990_01
特許番号
US04894359

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