Triethylamine → HCID 178418542、化合物

HRID 4675

反応式

HRID 4675 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 178418542HCID 178418542、化合物収率 31%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c3b37e31e5d14c2ab67233d672266e5e
出典データセット
uspto-grants-1988_02
特許番号
US04727073

関連ノート

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