Ethyl Bromide → HCID 20537465, 화합물

HRID 1155695노트

반응식

HRID 1155695 반응식
Cl.[NH:2]1[C:10]2[C:5](=[C:6]([C:11]3([OH:17])[CH2:16][CH2:15][CH2:14][NH:13][CH2:12]3)[CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3]1.C(=O)([O-])[O-].[Na+].[Na+].[CH2:24](Br)[CH3:25]>CN(C)C=O.O>[CH2:24]([N:13]1[CH2:14][CH2:15][CH2:16][C:11]([C:6]2[CH:7]=[CH:8][CH:9]=[C:10]3[C:5]=2[CH:4]=[CH:3][NH:2]3)([OH:17])[CH2:12]1)[CH3:25]

참가 물질

6

반응물 3

HCID 6332Ethyl BromideHCID 10340Sodium CarbonateHCID 12900686HCID 12900686, 화합물

생성물 1

HCID 20537465HCID 20537465, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 10 g of 3-(1H-indol-4-yl)-3-piperidinol hydrochloride in 200 ml of dimethylformamide was agitated for 4 hours under an inert atmosphere with 13.44 g of sodium carbonate and 4.2 ml of ethyl bromide. The mixture was taken up in water and was extracted with ethyl acetate. The organic phase was washed with water, dried, filtered and evaporated to dryness under reduced pressure at 50° C. The residue was purified by chromatography over silica and eluted with a 6-3-1 mixture of cyclohexane-chloroform-triethylamine to obtain 6.6 g of 1-ethyl-3-(1H-indol-4-yl)-3-piperidinol which was used as is for the following step.

후처리

  1. extractionwas extracted with ethyl acetate
  2. washThe organic phase was washed with water
  3. customdried
  4. filtrationfiltered
  5. customevaporated to dryness under reduced pressure at 50° C
  6. customThe residue was purified by chromatography over silica
  7. washeluted with a 6-3-1 mixture of cyclohexane-chloroform-triethylamine

출처 및 근거

ORD 기록
ord-095436143ccf47efa670d306dab120ff
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04332808

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