Water → HCID 20537467, 화합물

HRID 1155690노트

반응식

HRID 1155690 반응식
C(=O)([O-])[O-].[Na+].[Na+].[CH2:7](Br)[CH:8]=[CH2:9].Cl.[NH:12]1[C:20]2[C:15](=[C:16]([C:21]3([OH:27])[CH2:26][CH2:25][CH2:24][NH:23][CH2:22]3)[CH:17]=[CH:18][CH:19]=2)[CH:14]=[CH:13]1.O>CN(C)C=O.C(OCC)(=O)C>[CH2:7]([N:23]1[CH2:24][CH2:25][CH2:26][C:21]([C:16]2[CH:17]=[CH:18][CH:19]=[C:20]3[C:15]=2[CH:14]=[CH:13][NH:12]3)([OH:27])[CH2:22]1)[CH:8]=[CH2:9]

참가 물질

7

반응물 4

HCID 962WaterHCID 7841Allyl bromideHCID 10340Sodium CarbonateHCID 12900686HCID 12900686, 화합물

생성물 1

HCID 20537467HCID 20537467, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

22.9 g of sodium carbonate and 7.6 ml of allyl bromide were added to a mixture of 18 g of 3-(1H-indol-4-yl)-3-piperidinol hydrochloride in 350 ml of dimethylformamide and the mixture was stirred under an inert atmosphere at room temperature for 2 hours. Then, one liter of water and 500 ml of ethyl acetate were added thereto and the decanted organic phase was washed with water, dried and evaporated to dryness under reduced pressure. The 17 g of residue were chromatographed over silica gel and eluted with a 6-3-1 cyclohexanechloroform-triethylamine mixture to obtain 14 g of 1-(2-propenyl)-3-(1H-indol-4-yl)-3-piperidinol with an Rf=0.15.

후처리

  1. washthe decanted organic phase was washed with water
  2. customdried
  3. customevaporated to dryness under reduced pressure
  4. customThe 17 g of residue were chromatographed over silica gel
  5. washeluted with a 6-3-1 cyclohexanechloroform-triethylamine mixture

출처 및 근거

ORD 기록
ord-6651c45bc9224a1e81991c7b1f4e7489
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04332808

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