Potassium Hydroxide → HCID 13145802, 화합물

HRID 1074545노트

반응식

HRID 1074545 반응식
[OH-].[K+].[F:3][C:4]1[CH:5]=[C:6]([CH:16]=[CH:17][CH:18]=1)[CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1.Cl[CH2:20][CH2:21][CH2:22][N:23]1[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1>C(O)C>[F:3][C:4]1[CH:5]=[C:6]([CH:16]=[CH:17][CH:18]=1)[CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:20][CH2:21][CH2:22][N:23]2[CH2:28][CH2:27][O:26][CH2:25][CH2:24]2)=[CH:11][CH:10]=1

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 958344-(3-Chloropropyl)morpholineHCID 13145801HCID 13145801, 화합물

생성물 1

HCID 13145802HCID 13145802, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

To a solution of 0.56 g (0.01 mol) of potassium hydroxide in 18 ml of absolute ethanol are added 2.18 g (0.01 mol) of 4-(3-fluorobenzyloxy)phenol. There is then added a solution of 1.64 g (0.01 mol) of N-(3-chloropropyl)morpholine in 2 ml of absolute ethanol. The mixture is stirred at reflux for 24 hours, allowed to cool and then refrigerated. The solid which forms is collected by filtration, washed with absolute ethanol and dissolved in diethyl ether. The ethereal solution is washed consecutively with water (20 ml), 10% aqueous sodium hydroxide (3×15 ml) and water until neutral to litmus. The solution is dried over sodium sulfate, filtered and evaporated and recrystallized from diethyl ether-petroleum ether and from diethyl ether alone to yield N-[3-(4-{3-fluorobenzyloxy}phenoxy)propyl]morpholine.

후처리

  1. temperatureat reflux for 24 hours
  2. temperatureto cool
  3. filtrationThe solid which forms is collected by filtration
  4. washwashed with absolute ethanol
  5. dissolutiondissolved in diethyl ether
  6. washThe ethereal solution is washed consecutively with water (20 ml), 10% aqueous sodium hydroxide (3×15 ml) and water until neutral to litmus
  7. dry with materialThe solution is dried over sodium sulfate
  8. filtrationfiltered
  9. customevaporated
  10. customrecrystallized from diethyl ether-petroleum ether and from diethyl ether alone

출처 및 근거

ORD 기록
ord-c72717f097ab4d5d86c01c5367f111de
출처 데이터셋
uspto-grants-1983_07
특허 번호
US04393061

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