Methanol → 2,6-dimethyl-7a-undecyl-tetrahydro-2H-oxazolo[2,3-b]oxazole

HRID 2116743

반응식

HRID 2116743 반응식
[CH3:1][CH:2]([OH:9])[CH2:3][NH:4][CH2:5][CH:6]([OH:8])[CH3:7].[C:10](OC)(=O)[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21].CO>>[CH3:1][CH:2]1[O:9][C:21]2([CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH3:10])[O:8][CH:6]([CH3:7])[CH2:5][N:4]2[CH2:3]1

참가 물질

4

반응물 3

HCID 887MethanolHCID 8086Diisopropanolamine3회HCID 8139Methyl Laurate2회

생성물 1

HCID 692034952,6-dimethyl-7a-undecyl-tetrahydro-2H-oxazolo[2,3-b]oxazole

반응 조건

온도
230 °C

실험 절차

To a 1 liter stirred reactor, equipped with a distillation column, condenser, and graduated receiver, the following constituents were added: 261.2 g of diisopropanol amine (DIPA) and 432.0 g (98%) of methyl laurate. The contents were heated slowly to 230° C. under a nitrogen blanket. After 5.5 hours, 57 ml of methanol (0.72 equivalent) had come overhead. The pressure was then slowly lowered to strip out unreacted DIPA. At a batch temperature of 180° C. and a pressure of 293 Pa, a cut consisting of 79.7 g of DIPA and 87.8 g of methyl laurate was removed. The batch temperature was then raised to 200° C. and the pressure dropped to 267 Pa. During this period, a cut of 140.9 g of the amide acetal was recovered. This represents a 35.7% conversion of the methyl laurate to amide acetal.

후처리

  1. customequipped with a distillation column, condenser
  2. additionthe following constituents were added
  3. customAt a batch temperature of 180° C.
  4. customwas removed
  5. temperatureThe batch temperature was then raised to 200° C.
  6. additionthe pressure dropped to 267 Pa
  7. waitDuring this period
  8. customa cut of 140.9 g of the amide acetal was recovered

출처 및 근거

ORD 기록
ord-619dec1ca69149a4b70f3f0d560f1bfb
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07439354B2

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