Ethyl Bromide → HCID 20537465、化合物

HRID 1155695ノート

反応式

HRID 1155695 の反応式
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]

参加物

6

反応物 3

HCID 6332Ethyl BromideHCID 10340Sodium CarbonateHCID 12900686HCID 12900686、化合物

生成物 1

HCID 20537465HCID 20537465、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-095436143ccf47efa670d306dab120ff
出典データセット
uspto-grants-1982_06
特許番号
US04332808

反応ノート

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