Dimethylformamide → 1H-Indole, 5-chloro-3-(1-propyl-1,2,3,6-tetrahydro-4-pyridinyl)-, monohydrochloride

HRID 1277652노트

반응식

HRID 1277652 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][CH:6]=[C:5]2[C:11]1[CH2:12][CH2:13][NH:14][CH2:15][CH:16]=1.CN(C)C=O.C(=O)([O-])[O-].[Na+].[Na+].[CH2:28](I)[CH2:29][CH3:30]>O>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][CH:6]=[C:5]2[C:11]1[CH2:12][CH2:13][N:14]([CH2:28][CH2:29][CH3:30])[CH2:15][CH:16]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 10340Sodium CarbonateHCID 336431-IodopropaneHCID 30505325-chloro-3-(1,2,3,6-tetrahydropyridin-4-yl)-1H-indole

생성물 1

HCID 30557471H-Indole, 5-chloro-3-(1-propyl-1,2,3,6-tetrahydro-4-pyridinyl)-, monohydrochloride수율 112%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 9.28 g of 5-chloro-3-(1,2,3,6-tetrahydropyridin-4-yl)-1H-indole (prepared by the process of Belgium Pat. No. 858,101), 140 ml of dimethylformamide, 8.48 g of sodium carbonate and 4.67 g of propyl iodide was stirred for 5 hours at room temperature under an inert atmosphere and was then poured with stirring into 1.4 liters of water after which crystallization occured. The mixture was filtered and the recovered product was rinsed with water and dried under reduced pressure in the presence of a dehydrating agent. The product was crystallized from ethanol to obtain 6.95 g of 5-chloro-3-(1-propyl-1,2,3,6-tetrahydropyridin-4-yl)-1H-indole hydrochloride melting at 229°-230° C.

후처리

  1. customprepared by the process of Belgium Pat
  2. additionwas then poured
  3. customafter which crystallization
  4. filtrationThe mixture was filtered
  5. washthe recovered product was rinsed with water
  6. customdried under reduced pressure in the presence of a dehydrating agent
  7. customThe product was crystallized from ethanol

출처 및 근거

ORD 기록
ord-9c86e559e4bd4be998d1e1f3f1ad7528
출처 데이터셋
uspto-grants-1981_07
특허 번호
US04278677

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