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Formaldehyde → 3-(beta-Hydroxypropyl)tetrahydro-1,3-oxazine

HRID 2398035
노트
인쇄 미리보기

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HRID 2398035 반응식
[OH:1][CH2:2][CH2:3][CH2:4][NH:5][CH2:6]CCO.C=[O:11].[C:12]1([CH3:18])[CH:17]=CC=CC=1>>[OH:11][CH:12]([CH3:18])[CH2:17][N:5]1[CH2:4][CH2:3][CH2:2][O:1][CH2:6]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 712Formaldehyde2회HCID 1140TolueneHCID 106986Dipropanolamine

생성물 1

HCID 214343563-(beta-Hydroxypropyl)tetrahydro-1,3-oxazine

반응 조건

온도
90 °C

실험 절차

To a glass reaction vessel equipped with stirrer, thermometer, and condenser fitted with a water trap is added di-(3-hydroxypropyl) amine (3.0 mole, 399 g.) and toluene (500 g.). Paraformaldehyde (3.15 mole, 90% pure, 105 g.) is weighed out and about 1/3 is added to the amine solution. The resulting mixture is stirred and heated to 90° C. while slowly adding the remaining paraformaldehyde in about 70 minutes. The reaction is heated to reflux and the water separated. After 4 hours, a total of 63 ml. of water is removed. Toluene is removed at reduced pressure. The residue is distilled at high vacuum to yield 3-(β-hydroxypropyl)tetrahydro-1,3-oxazine.

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

후처리

  1. customTo a glass reaction vessel
  2. customequipped with stirrer
  3. customthermometer, and condenser fitted with a water trap
  4. temperatureThe reaction is heated
  5. temperatureto reflux
  6. customthe water separated
  7. customof water is removed
  8. customToluene is removed at reduced pressure
  9. distillationThe residue is distilled at high vacuum

출처 및 근거

ORD 기록
ord-610d73d0d4ef4c908c5295fff4193b88
출처 데이터셋
uspto-grants-1977_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04024117

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