ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Water → 3-[2-(1,2,5,6-Tetrahydro-4-pyridyl)-ethyl]-indole

HRID 1632976
ノート
印刷プレビュー

反応式

HRID 1632976 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([CH2:7][CH2:8][C:9]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[NH:11][CH:10]=2)=[CH:3][CH:2]=1.[Na].O>C(O)CCC>[NH:1]1[CH2:6][CH2:5][C:4]([CH2:7][CH2:8][C:9]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[NH:11][CH:10]=2)=[CH:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 279343-(2-(4-Pyridyl)ethyl)indoleHCID 5360545Sodium2 回

生成物 1

HCID 132059893-[2-(1,2,5,6-Tetrahydro-4-pyridyl)-ethyl]-indole収率 24.8%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

A solution of 10.3 g of 3-[2-(4-pyridyl)-ethyl]-indole (prepared according to U.S. Pat. No. 3,300,506) in 400 ml n-butanol was heated, under nitrogen, at a temperature of approximately 90° C. Thereafter, 8 g of sodium were added portionwise while agitating magnetically and the temperature was raised to and maintained at about 110° C. until the sodium disappeared. Once the ambient temperature had been restored, the solution was poured into 400 ml water, the organic phase washed with water until it became neutral and then was dried over sodium sulfate and evaporated under vacuum. The evaporation residue was mixed with 25 ml absolute ethanol and purified by means of chromatography over silica gel, (eluant: ethanol-diethylamine=40-1). Following two processes of crystallization in methanol, 2.6 g of 3-[2-(1,2,5,6-tetrahydro-4-pyridyl)-ethyl]-indole were obtained, which melted at 155° C.

後処理

  1. temperaturethe temperature was raised to and
  2. customthe ambient temperature
  3. washthe organic phase washed with water until it
  4. dry with materialwas dried over sodium sulfate
  5. customevaporated under vacuum
  6. additionThe evaporation residue was mixed with 25 ml absolute ethanol
  7. custompurified by means of chromatography over silica gel, (eluant: ethanol-diethylamine=40-1)
  8. customtwo processes of crystallization in methanol

出典と根拠

ORDレコード
ord-77d1fc94d2ba4096a0ffb553dc0d9bce
出典データセット
uspto-grants-1984_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04478841

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート