Tetrahydrofuran → Bis(p-dimethylaminophenyl)Methoxy Acetic Acid, Benzyl Ester

HRID 66930

反応式

HRID 66930 の反応式
[CH3:1][N:2]([C:4]1[CH:20]=[CH:19][C:7]([CH:8]([OH:18])[C:9]2[CH:14]=[CH:13][C:12]([N:15]([CH3:17])[CH3:16])=[CH:11][CH:10]=2)=[CH:6][CH:5]=1)[CH3:3].COC.[C:24]([O:28][CH2:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)(=[O:27])[CH2:25]O.O1CCCC1>CS(O)(=O)=O.CCCCCC>[CH3:17][N:15]([CH3:16])[C:12]1[CH:13]=[CH:14][C:9]([CH:8]([C:7]2[CH:19]=[CH:20][C:4]([N:2]([CH3:1])[CH3:3])=[CH:5][CH:6]=2)[O:18][CH2:25][C:24]([O:28][CH2:29][C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)=[O:27])=[CH:10][CH:11]=1

参加物

7

反応物 4

HCID 8028TetrahydrofuranHCID 8254Dimethyl EtherHCID 927424,4'-Bis(dimethylamino)benzhydrolHCID 561337Benzyl 2-hydroxyacetate

生成物 1

HCID 131712798Bis(p-dimethylaminophenyl)Methoxy Acetic Acid, Benzyl Ester

試薬・触媒・溶媒 2

HCID 6395Methanesulfonic Acid触媒HCID 8058Hexane溶媒

実験手順

A solution of 4,4'-bis(N,N-dimethylamino)benzhydrol, methyl ether (11.0 g, 0.039 mole), benzyl glycolate (6.6 g, 0.039 mole), 90 ml of tetrahydrofuran, 200 ml of hexane, and 10 drops of methanesulfonic acid was refluxed for 6 hours, replacing solvent as distillate was removed; then, 10 drops of tetramethylguanidine was added to discharge the color and the reaction mixture was filtered hot and cooled. A white solid formed which was filtered, washed with petroleum ether and then recrystallized from 4/1 hexane/acetone. The resulting white crystalline product had a mp 101.8°-103° C.

後処理

  1. customwas removed
  2. additionthen, 10 drops of tetramethylguanidine was added
  3. filtrationthe reaction mixture was filtered hot
  4. temperaturecooled
  5. customA white solid formed which
  6. filtrationwas filtered
  7. washwashed with petroleum ether
  8. customrecrystallized from 4/1 hexane/acetone

出典と根拠

ORDレコード
ord-c8c7ee5975cb486097236de1755ecc83
出典データセット
uspto-grants-1982_08
特許番号
US04343939

関連ノート

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