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

HRID 66929

반응식

HRID 66929 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 6395Methanesulfonic Acid촉매HCID 8058Hexane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-aedb3f7bf82141bca0c692617ca9a875
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04343939

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