Water → Piperazine, 1-(3-chloropropyl)-4-(3-(trifluoromethyl)phenyl)-

HRID 126779

반응식

HRID 126779 반응식
[OH-].[Na+].O.Cl.[F:5][C:6]([F:20])([F:19])[C:7]1[CH:8]=[C:9]([N:13]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)[CH:10]=[CH:11][CH:12]=1.Br[CH2:22][CH2:23][CH2:24][Cl:25]>CC(C)=O>[F:20][C:6]([F:5])([F:19])[C:7]1[CH:8]=[C:9]([N:13]2[CH2:18][CH2:17][N:16]([CH2:22][CH2:23][CH2:24][Cl:25])[CH2:15][CH2:14]2)[CH:10]=[CH:11][CH:12]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 80061-Bromo-3-chloropropaneHCID 14798Sodium HydroxideHCID 3084246TFMPP hydrochloride

생성물 1

HCID 3060362Piperazine, 1-(3-chloropropyl)-4-(3-(trifluoromethyl)phenyl)-

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of 7.36 g. (0.184 mole) of sodium hydroxide in 75 ml. of water and 75 ml. of acetone there is added 19.02 g. (0.074 mole) of 1-[3-(trifluoromethyl)phenyl]piperazine hydrochloride and 11.59 g. (0.074 mole) of 1-bromo-3-chloropropane, and the resulting mixture is stirred at 27° for 18 hrs. The organic layer is then separated and concentrated to an oil under reduced pressure. The oil is treated with hot (85°) 6 N HCl until solution is complete, and the resulting solution is filtered and stored at 5° for 18 hrs. The precipitate which forms is collected on a filter to afford 14.73 g. (66%) of the hydrochloride salt of the product, m.p. 190°-192°.

후처리

  1. customThe organic layer is then separated
  2. concentrationconcentrated to an oil under reduced pressure
  3. additionThe oil is treated with hot (85°) 6 N HCl until solution
  4. filtrationthe resulting solution is filtered
  5. customThe precipitate which forms is collected on
  6. filtrationa filter
  7. customto afford 14.73 g

출처 및 근거

ORD 기록
ord-5ca3d4c1e7d04bb191f7c2ba1b7a79c2
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254124

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