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

HRID 1060207

反応式

HRID 1060207 の反応式
[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]

参加物

4

反応物 2

HCID 17857Isophorone diamineHCID 522677Isobutyl acetoacetate

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒3 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-01d6ba5754764b41bbc2f4b9915834c2
出典データセット
uspto-grants-2003_02
特許番号
US06521716B1

関連ノート

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