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

HRID 2354030ノート

反応式

HRID 2354030 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-a461e8d53b7c49258e679463feb20bd6
出典データセット
uspto-grants-2010_07
特許番号
US07750156B2

反応ノート

読み込み中…