Isophorone diamine → HCID 18667850, 화합물

HRID 1060203

반응식

HRID 1060203 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.[CH3:13][C:14]1[O:20]C(C)(C)[O:18][C:16](=O)[CH:15]=1>C1(C)C(C)=CC=CC=1>[C:16]([NH:11][CH:4]1[CH2:3][C:2]([CH3:12])([CH3:1])[CH2:7][C:6]([CH2:9][NH:10][C:16](=[O:18])[CH2:15][C:14]([CH3:13])=[O:20])([CH3:8])[CH2:5]1)(=[O:18])[CH2:15][C:14]([CH3:13])=[O:20]

참가 물질

4

반응물 2

HCID 17857Isophorone diamineHCID 793682,2,6-Trimethyl-4H-1,3-dioxin-4-one

생성물 1

HCID 18667850HCID 18667850, 화합물수율 98%

시약·촉매·용매 1

HCID 7237O-Xylene용매2회

반응 조건

온도
120 °C

실험 절차

To isophoronediamine (139.24 g, 0.819 mol) in xylene (525 ml) at 120° C. was added with stirring 2,2,6-trimethyl-1,3-dioxen-4-one (232.51 g, 1.637 mol) in xylene (525 ml) over 10 minutes, during which the temperature decreased to 103° C. Vigorous effervescence and distillation of acetone (through a Vigreux column) immediately commenced. Pot temperature was increased to 120° C. over 15 minutes, and to 139° C. over a further 30 minutes, with collection of acetone distillate. After cooling to 58° C., supernatant solution was separated from deposited gum, which was dissolved in dichloromethane. Removal of solvent from combined solutions and drying (91° C./100 Pa) gave 1-acetoacetamido-3-acetoacetamidomethyl-3,5,5-trimethylcyclohexane (270.21 g, 98%), (AAMTCH), which was crushed to a light yellow powder, mp 144-147° C. (mixture of E and Z isomers), and identified by 1H-NMR, 13C-NMR, FT-IR and Raman spectra.

후처리

  1. customdecreased to 103° C
  2. distillationVigorous effervescence and distillation of acetone (through a Vigreux column)
  3. distillationwith collection of acetone distillate
  4. temperatureAfter cooling to 58° C.
  5. customsupernatant solution was separated
  6. dissolutionwas dissolved in dichloromethane
  7. customRemoval of solvent from combined solutions
  8. customdrying (91° C./100 Pa)

출처 및 근거

ORD 기록
ord-1495e1282f644d5ebefce3b5ac4853f1
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06521716B1

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