Water → 1-(Benzoyloxy)-2-methyl-2-propanaminium chloride

HRID 426852노트

반응식

HRID 426852 반응식
[ClH:1].[C:2]1([C:8]2[O:9][CH2:10][C:11]([CH3:14])([CH3:13])[N:12]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH2:15]>Cl.O1CCCC1>[ClH:1].[C:8]([O:9][CH2:10][C:11]([NH2:12])([CH3:14])[CH3:13])(=[O:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 2

HCID 962WaterHCID 12220134Oxazole, 4,5-dihydro-4,4-dimethyl-2-phenyl-, hydrochloride

생성물 1

HCID 546091031-(Benzoyloxy)-2-methyl-2-propanaminium chloride

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 8028Tetrahydrofuran용매

실험 절차

To 8.7 g (0.041 mol) 2-phenyl-4,4-dimethyl-1,3-oxazoline hydrochloride suspended in 120 ml anhydrous hydrogen chloride in tetrahydrofuran (1 M) was added 3.6 ml (0.20 mol) water. The mixture was warmed to cause solution and heated under reflux with stirring for 1 hour. The tetrahydrofuran was removed under reduced pressure to afford a nearly colorless oil which crystallized at 0° following the addition of anhydrous ether. The solid was triturated with anhydrous ether overnight and isolated by filtration under a nitrogen atmosphere. After drying in vacuo over calcium sulfate, 6.9 g (0.30 mol), 73%, 2-amino-2-methyl-1-propyl benzoate hydrochloride was obtained as a white solid, mp 225°-228° (dec.) acetone:hexane, ir (KBr) 1725 (c=o) cm-1, pmr (D2O) δ 1.50 (s, 6H), 4.4 (s, 2H) and 7.0-8.3 (m, 5H) ppm.

후처리

  1. temperatureThe mixture was warmed
  2. temperatureheated
  3. temperatureunder reflux
  4. customThe tetrahydrofuran was removed under reduced pressure
  5. customto afford a nearly colorless oil which
  6. customcrystallized at 0°
  7. additionthe addition of anhydrous ether
  8. customThe solid was triturated with anhydrous ether overnight
  9. customisolated by filtration under a nitrogen atmosphere
  10. dry with materialAfter drying in vacuo over calcium sulfate, 6.9 g (0.30 mol), 73%

출처 및 근거

ORD 기록
ord-297ad8181b944ee495c1662234022122
출처 데이터셋
uspto-grants-1979_10
특허 번호
US04171452

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