Isophorone diamine → 1-(1-Isobutoxycarbonyl-2-prop-1-enylamino)-3-(1-isobutoxycarbonyl-2-prop-1-enylaminomethyl)-3,5,5-trimethylcyclohexane

HRID 1060207

반응식

HRID 1060207 반응식
[CH3:1][C:2]1([CH3:12])[CH2:7][C:6]([CH2:9][NH2:10])([CH3:8])[CH2:5][CH:4]([NH2:11])[CH2:3]1.[C:13]([O:19][CH2:20][CH:21]([CH3:23])[CH3:22])(=[O:18])[CH2:14][C:15]([CH3:17])=O>CO>[CH2:20]([O:19][C:13]([CH:14]=[C:15]([NH:11][CH:4]1[CH2:3][C:2]([CH3:12])([CH3:1])[CH2:7][C:6]([CH:9]([NH:10][C:15]([CH3:17])=[CH2:14])[C:13]([O:19][CH2:20][CH:21]([CH3:23])[CH3:22])=[O:18])([CH3:8])[CH2:5]1)[CH3:17])=[O:18])[CH:21]([CH3:23])[CH3:22]

참가 물질

4

반응물 2

HCID 17857Isophorone diamineHCID 522677Isobutyl acetoacetate

생성물 1

HCID 698581921-(1-Isobutoxycarbonyl-2-prop-1-enylamino)-3-(1-isobutoxycarbonyl-2-prop-1-enylaminomethyl)-3,5,5-trimethylcyclohexane수율 100%

시약·촉매·용매 1

HCID 887Methanol용매3회

실험 절차

To isophoronediamine (139.23 g, 0.819 mol) in methanol (700 ml) was slowly added with stirring isobutyl acetoacetate (262.31 g, 1.660 mol) in methanol (700 ml) over 45 minutes, during which the temperature increased from 22° C. to 30° C. The reaction mixture was allowed to stand at 21° C. overnight (15 h). Further methanol was added, and removal of solvent and drying (91° C./100 Pa) gave 1-(1-isobutoxycarbonyl-2-prop-1-enylamino)-3-(1-isobutoxycarbonyl-2-prop-1-enylaminomethyl)-3,5,5-trimethylcyclohexane (IIMTCH) as a clear light yellow viscous syrup (366.80 g, 100%), which set to a soft gum on standing and was identified by 1H-NMR, 13C-NMR, FT-IR and Raman spectra.

후처리

  1. temperatureincreased from 22° C. to 30° C
  2. custom(15 h)
  3. customremoval of solvent
  4. customdrying (91° C./100 Pa)

출처 및 근거

ORD 기록
ord-01d6ba5754764b41bbc2f4b9915834c2
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06521716B1

연결된 노트

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