Triethylamine → 1-(4-Hydroxyphenyl)-4-(4-trifluoromethoxyphenoxy)piperidine p-toluenesulfonate

HRID 2354030노트

반응식

HRID 2354030 반응식
[F:1][C:2]([F:18])([F:17])[O:3][C:4]1[CH:16]=[CH:15][C:7]([O:8][CH:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[CH:6][CH:5]=1.[C:19]1(=O)[CH2:24][CH2:23][C:22](=[O:25])[CH2:21][CH2:20]1.C(N(CC)CC)C.O.[C:35]1([CH3:45])[CH:40]=[CH:39][C:38]([S:41]([OH:44])(=[O:43])=[O:42])=[CH:37][CH:36]=1>C(O)C>[C:35]1([CH3:45])[CH:36]=[CH:37][C:38]([S:41]([OH:44])(=[O:42])=[O:43])=[CH:39][CH:40]=1.[OH:25][C:22]1[CH:23]=[CH:24][C:19]([N:12]2[CH2:11][CH2:10][CH:9]([O:8][C:7]3[CH:15]=[CH:16][C:4]([O:3][C:2]([F:1])([F:17])[F:18])=[CH:5][CH:6]=3)[CH2:14][CH2:13]2)=[CH:20][CH:21]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 125111,4-CyclohexanedioneHCID 521998p-Toluenesulfonic acid monohydrateHCID 161154394-[4-(Trifluoromethoxy)phenoxy]piperidine

생성물 1

HCID 866152441-(4-Hydroxyphenyl)-4-(4-trifluoromethoxyphenoxy)piperidine p-toluenesulfonate수율 63.75%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

4.00 g of 4-(4-trifluoromethoxyphenoxy)piperidine, 2.575 g of 1,4-cyclohexanedione and 2.16 ml of triethylamine were heated in 60 ml of ethanol and reacted at 50° C. to 60° C. for 6 hours. After the completion of the reaction, the reaction mixture was concentrated under reduced pressure and ethyl acetate was added thereto to prepare an ethyl acetate solution, to which 4.37 g of p-toluenesulfonic acid monohydrate was added. After leaving at room temperature for 30 minutes, the precipitate was filtrated, washed with ethyl acetate and air-dried, and 5.116 g of 1-(4-hydroxyphenyl)-4-(4-trifluoromethoxyphenoxy)piperidine p-toluenesulfonate was obtained (yield 63.75%).

후처리

  1. customreacted at 50° C. to 60° C. for 6 hours
  2. customAfter the completion of the reaction
  3. concentrationthe reaction mixture was concentrated under reduced pressure and ethyl acetate
  4. additionwas added
  5. customto prepare an ethyl acetate solution
  6. customAfter leaving at room temperature for 30 minutes
  7. filtrationthe precipitate was filtrated
  8. washwashed with ethyl acetate
  9. customair-dried

출처 및 근거

ORD 기록
ord-a461e8d53b7c49258e679463feb20bd6
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07750156B2

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