Triethylamine → HCID 178418542, 화합물

HRID 4675

반응식

HRID 4675 반응식
[C:1]([C:4](=[CH:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[CH:10]=1)[C:5]([CH3:7])=[O:6])(=O)[CH3:2].Cl.[C:19]([NH2:27])(=[NH:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C(N(CC)CC)C.C(OCC)(=O)C>C(O)CCC>[C:5]([C:4]1[CH:8]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[CH:10]=2)[NH:27][C:19]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[N:26][C:1]=1[CH3:2])(=[O:6])[CH3:7]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 80289Benzamidine, hydrochlorideHCID 959903-((3-Nitrophenyl)methylene)-2,4-pentanedione

생성물 1

HCID 178418542HCID 178418542, 화합물수율 31%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

A mixture of 1-acetyl-1-(3-nitrobenzyliden)acetone (10 g), benzamidine hydrochloride (8.06 g) and triethylamine (8.4 ml) in n-butanol (100 ml) was refluxed for 2 hours. The reaction mixture was added ethyl acetate (100 ml), washed with water (100 ml) and 5% hydrochloric acid (100 ml) successively. The solvent was evaporated and the residue was stirred with ethyl acetate (100 ml) for 1 hour. The crystals were collected by filtration, added a mixture of chloroform (100 ml) and water (100 ml) and adjusted to pH 8.5 by saturated potassium carbonate. The organic layer was evaporated in vacuo to give 5-acetyl-4-methyl-6-(3-nitrophenyl)-2-phenyl-1,6-dihydropyrimidine (4.46 g).

후처리

  1. temperaturewas refluxed for 2 hours
  2. washwashed with water (100 ml) and 5% hydrochloric acid (100 ml) successively
  3. customThe solvent was evaporated
  4. filtrationThe crystals were collected by filtration
  5. additionadded
  6. additiona mixture of chloroform (100 ml) and water (100 ml)
  7. customThe organic layer was evaporated in vacuo

출처 및 근거

ORD 기록
ord-c3b37e31e5d14c2ab67233d672266e5e
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04727073

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