Ethyl Acetate → Benzyl 5,6-dihydro-1-methyl-2-phenyl-4H-1,3,4-triazine-5-carboxylate

HRID 1651462ノート

反応式

HRID 1651462 の反応式
I.C[N:3]([C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[NH:6])[NH2:4].Br[C:14](=[CH2:25])[C:15]([O:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:16].N12CCCC1=NCC[CH2:27]2.C(OCC)(=O)C>CN(C)C=O.C1C=CC=CC=1>[CH3:27][N:6]1[CH2:25][CH:14]([C:15]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:16])[NH:4][N:3]=[C:5]1[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参加物

7

反応物 4

HCID 8857Ethyl AcetateHCID 763491,5-Diazabicyclo(4.3.0)non-5-eneHCID 13327794N-methylbenzenecarboximidohydrazide hydroiodideHCID 13443472Benzyl 2-bromoprop-2-enoate

生成物 1

HCID 23051225Benzyl 5,6-dihydro-1-methyl-2-phenyl-4H-1,3,4-triazine-5-carboxylate

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 6228Dimethylformamide溶媒2 回

実験手順

Benzenecarboximidic acid-N-methyl hydrazide monohydroiodide (0.43 g) in dry dimethylformamide (10 ml) and benzyl 2-bromo-prop-2-enoate (0.41 g) in benzene (2.5 ml) were cooled to 0° and stirred together under an atmosphere of nitrogen. A solution of 1,5-diazabicyclo[4.3.0]non-5-ene (0.4 ml) in dimethylformamide (5 ml) was added gradually and the mixture was stirred at 0° for a further 20 minutes. Ethyl acetate (100 ml) was added and the mixture was washed with brine (30 ml) and dried over magnesium sulphate. The solvent was removed at reduced pressure to yield the sub-title product (0.46 g) as an orange oil.

後処理

  1. stirringthe mixture was stirred at 0° for a further 20 minutes
  2. washthe mixture was washed with brine (30 ml)
  3. dry with materialdried over magnesium sulphate
  4. customThe solvent was removed at reduced pressure

出典と根拠

ORDレコード
ord-88da4b961b824318bf89175698c207d7
出典データセット
uspto-grants-1990_05
特許番号
US04927822

反応ノート

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