Tetrahydrofuran → 4-[[Bis(p-dimethylaminophenyl)methoxy]acetyl]Morpholine

HRID 66929

反応式

HRID 66929 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].[CH3:21][O:22][CH3:23].[O:24]1CC[CH2:26][CH2:25]1.[CH3:29][N:30](C)[C:31](=N)N(C)C>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][CH2:26][C:25]([N:30]2[CH2:31][CH2:23][O:22][CH2:21][CH2:29]2)=[O:24])=[CH:10][CH:11]=1

参加物

7

反応物 4

HCID 8028TetrahydrofuranHCID 8254Dimethyl EtherHCID 664601,1,3,3-TetramethylguanidineHCID 927424,4'-Bis(dimethylamino)benzhydrol

生成物 1

HCID 204880364-[[Bis(p-dimethylaminophenyl)methoxy]acetyl]Morpholine

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 (9.0 g, 0.032 mole), glycol morpholinamide (4.6 g, 0.032 mole), 150 ml of tetrahydrofuran, 250 ml of n-hexane and 4 drops of methanesulfonic acid was refluxed for about 8 hours, during which time an additional 200 ml of solvent was added. The volume was reduced to 200 ml and the color was discharged with tetramethylguanidine. The solution was filtered hot and then cooled to precipitate a white solid. The solid was recrystallized from 350 ml of methyl cyclohexane to give 4.9 g of blue crystals; mp 147.8°-150° C.

後処理

  1. additionwas added
  2. filtrationThe solution was filtered hot
  3. temperaturecooled
  4. customto precipitate a white solid
  5. customThe solid was recrystallized from 350 ml of methyl cyclohexane

出典と根拠

ORDレコード
ord-aedb3f7bf82141bca0c692617ca9a875
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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