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Ethyl orthoformate → 8-Benzyl-1-(3-methyl-phenyl)-1,3,8-triazaspiro[4,5]dec-2-en-4-one

HRID 1638217
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HRID 1638217 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]2([C:22]([NH2:24])=[O:23])[CH2:14][CH2:13][N:12]([CH2:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:11][CH2:10]2)[CH:5]=[CH:6][CH:7]=1.[CH:25](OCC)(OCC)OCC>>[CH2:15]([N:12]1[CH2:11][CH2:10][C:9]2([N:8]([C:4]3[CH:5]=[CH:6][CH:7]=[C:2]([CH3:1])[CH:3]=3)[CH:25]=[N:24][C:22]2=[O:23])[CH2:14][CH2:13]1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 31214Ethyl orthoformateHCID 211931981-Benzyl-4-(3-methylphenylamino)isonipecotamide

생성물 1

HCID 212683698-Benzyl-1-(3-methyl-phenyl)-1,3,8-triazaspiro[4,5]dec-2-en-4-one

반응 조건

온도
150 °C

실험 절차

4-(3-methyl-phenyl-amino)-1-(phenylmethyl)-4-piperidine-carboxamide (12.94 g) was dissolved in 80 ml triethyl orthoformate and stirred at 150° C. for 66 hours. After cooling to 0° C., the reaction mixture was filtered and the light brown powder washed with ether to yield 8-benzyl-1-(3-methyl-phenyl)-1,3,8-triazaspiro[4,5]dec-2-en-4-one (2.1g). M.p. 301.5-302.6° C.

후처리

  1. temperatureAfter cooling to 0° C.
filtration
the reaction mixture was filtered
  • washthe light brown powder washed with ether
  • 출처 및 근거

    ORD 기록
    ord-d1b028fd2db2434c8de30b87c84c19eb
    출처 데이터셋
    uspto-grants-2000_03
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06043366

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