Triethylamine → 2-Trifluoromethyl-10-[3-(4-beta-{2-methylheptanoyloxy}ethoxypiperidino)-propyl]-phenothiazine

HRID 329045

반응식

HRID 329045 반응식
[F:1][C:2]([F:31])([F:30])[C:3]1[CH:16]=[CH:15][C:14]2[S:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[N:6]([CH2:17][CH2:18][CH2:19][N:20]3[CH2:25][CH2:24][CH:23]([O:26][CH2:27][CH2:28][OH:29])[CH2:22][CH2:21]3)[C:5]=2[CH:4]=1.C(N(CC)CC)C.[CH3:39][CH:40]([CH2:44][CH2:45][CH2:46][CH2:47][CH3:48])[C:41](Cl)=[O:42]>C1C=CC=CC=1>[F:31][C:2]([F:30])([F:1])[C:3]1[CH:16]=[CH:15][C:14]2[S:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[N:6]([CH2:17][CH2:18][CH2:19][N:20]3[CH2:21][CH2:22][CH:23]([O:26][CH2:27][CH2:28][O:29][C:41](=[O:42])[CH:40]([CH3:39])[CH2:44][CH2:45][CH2:46][CH2:47][CH3:48])[CH2:24][CH2:25]3)[C:5]=2[CH:4]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 218089FlupimazineHCID 142345192-Methylheptanoyl chloride

생성물 1

HCID 537215472-Trifluoromethyl-10-[3-(4-beta-{2-methylheptanoyloxy}ethoxypiperidino)-propyl]-phenothiazine수율 30%

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

13.55 g of 2-trifluoromethyl-10-[3-(4-β-hydroxyethoxypiperidino)-propyl]-phenothiazine (prepared by Example XLIII), 5.4 ml of triethylamine and 100 ml of anhydrous benzene were added to a flask and a solution of 5.7 g of 2-methyl-heptanoic acid chloride in 50 ml of anhydrous benzene was added thereto. The mixture was agitated at room temperature for 24 hours and then the precipitate formed was removed by filtration. The benzene filtrate was washed with an aqueous solution of sodium bicarbonate, then with water. After drying and concentration of the benzene solution, the resulting oil was purified by chromatography on silica gel. After elution with ethanol and evaporation of the solvent, 5.2 g of 2-trifluoromethyl-10-[3-(4-β-{2-methylheptanoyloxy}ethoxypiperidino)-propyl]-phenothiazine as a clear oil were obtained.

후처리

  1. customthe precipitate formed
  2. customwas removed by filtration
  3. washThe benzene filtrate was washed with an aqueous solution of sodium bicarbonate
  4. customAfter drying
  5. customconcentration of the benzene solution, the resulting oil was purified by chromatography on silica gel
  6. washAfter elution
  7. customwith ethanol and evaporation of the solvent

출처 및 근거

ORD 기록
ord-f1c30b42051d48ec83d999ce52d27245
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04018922

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