Triethylamine → {2-[3-(1,1-Dimethylundecyl)ureido]-4-methoxy-6-tert-butylphenoxy}methoxymethane

HRID 1457574노트

반응식

HRID 1457574 반응식
C[C:2]([CH3:16])([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])[C:3](O)=O.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:24])C=CC=CC=1.C([N:36]([CH2:39]C)CC)C.[NH2:41][C:42]1[CH:51]=[C:50]([O:52][CH3:53])[CH:49]=[C:48]([C:54]([CH3:57])([CH3:56])[CH3:55])[C:43]=1[O:44][CH2:45][O:46][CH3:47]>O.C1C=CC=CC=1>[CH3:16][C:2]([NH:36][C:39](=[O:24])[NH:41][C:42]1[CH:51]=[C:50]([O:52][CH3:53])[CH:49]=[C:48]([C:54]([CH3:57])([CH3:56])[CH3:55])[C:43]=1[O:44][CH2:45][O:46][CH3:47])([CH3:3])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15]

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 42657262,2-Dimethyldodecanoic acidHCID 18765846(2-Amino-4-methoxy-6-tert-butylphenoxy)methoxymethane

생성물 1

HCID 22099452{2-[3-(1,1-Dimethylundecyl)ureido]-4-methoxy-6-tert-butylphenoxy}methoxymethane

시약·촉매·용매 2

HCID 241Benzene용매2회HCID 962Water용매

실험 절차

A mixture of 5 g of 2,2-dimethyllauric acid, 4.72 ml of diphenylphosphorylazide (DPPA), 3.36 ml of triethylamine and 80 ml of benzene was refluxed for one hour. After cooling, a mixed solution of 5.763 g of (2-amino-4-methoxy-6-tert-butylphenoxy)methoxymethane and 20 ml of benzene was added dropwise to the above mixture. The resulting mixture was stirred at room temperature for one hour and then under reflux for 10 hours. Water was added to the reaction mixture, and the reaction mixture was extracted with ethyl acetate. The extract was washed and dried, and the solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography (solvent; hexane:ethyl acetate=4:1) and the product was recrystallized from hexane to give 2.89 g of {2-[3-(1,1-dimethylundecyl)ureido]-4-methoxy-6-tert-butylphenoxy}methoxymethane (melting point: 83°-85° C.).

후처리

  1. temperaturewas refluxed for one hour
  2. temperatureAfter cooling
  3. temperatureunder reflux for 10 hours
  4. extractionthe reaction mixture was extracted with ethyl acetate
  5. washThe extract was washed
  6. customdried
  7. customthe solvent was removed under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (solvent; hexane:ethyl acetate=4:1)
  9. customthe product was recrystallized from hexane

출처 및 근거

ORD 기록
ord-18e8b5c3d7bc4257a1aa16d682bbc4bf
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05849732

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