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

HRID 1651462노트

반응식

HRID 1651462 반응식
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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 241Benzene용매HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-88da4b961b824318bf89175698c207d7
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04927822

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