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Hydrochloric Acid → (S)-3-(2-(4-phenyl-4-carboxypiperidin-1-yl)ethyl)-3-(3,4-dichlorophenyl)pyrrolidine

HRID 1601448
ノート
印刷プレビュー

反応式

HRID 1601448 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([CH2:28][CH2:29][N:30]3[CH2:35][CH2:34][C:33]([C:39]4[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=4)([C:36](N)=[O:37])[CH2:32][CH2:31]3)[CH2:13][CH2:12][N:11](C(=O)C3C=C(OC)C(OC)=C(OC)C=3)[CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].[O:45]1CCOCC1.Cl>O>[C:39]1([C:33]2([C:36]([OH:45])=[O:37])[CH2:34][CH2:35][N:30]([CH2:29][CH2:28][C@:9]3([C:4]4[CH:5]=[CH:6][C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=4)[CH2:13][CH2:12][NH:11][CH2:10]3)[CH2:31][CH2:32]2)[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=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 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 98741684-Phenyl-1-[2-[3-(3,4-dichlorophenyl)-1-(3,4,5-trimethoxybenzoyl)pyrrolidin-3-yl]ethyl]piperidine-4-carboxamide

生成物 1

HCID 53783991(S)-3-(2-(4-phenyl-4-carboxypiperidin-1-yl)ethyl)-3-(3,4-dichlorophenyl)pyrrolidine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Combine (+)-1-(2-(3-(3,4-dichlorophenyl)-1-(3,4,5-trimethoxybenzoyl)-pyrrolidin-3-yl)-ethyl)-4-phenylpiperidine-4-carboxylic acid amide prepared by the method of U.S. Pat. No. 5,635,510, issued Jun. 3, 1997 (200 g, 300 mmol), dioxane (400 mL), concentrated aqueous hydrochloric acid (400 mL), and water (400 mL). Heat to reflux. After 26 hours, cool to ambient temperature and concentrate the reaction mixture in vacuo at about 60° C. to a volume of about 700 mL. Add water (400 mL) and extract with 9/1 ethyl acetate/hexaneo Separate the layers and extract the aqueous layer twice with 1/1 ethyl acetate/hexane. Adjust the pH of the aqueous layer to about 7 using sodium hydroxide to form a solid. Filter and dry to give (S)-3-(2-(4-phenyl-4-carboxypiperidin-1-yl)ethyl)-3-(3,4-dichlorophenyl)pyrrolidine.

後処理

  1. temperatureHeat to reflux
  2. concentrationconcentrate the reaction mixture in vacuo at about 60° C. to a volume of about 700 mL
  3. extractionAdd water (400 mL) and extract with 9/1 ethyl acetate/hexaneo
  4. customSeparate the layers
  5. extractionextract the aqueous layer twice with 1/1 ethyl acetate/hexane
  6. customto form a solid
  7. filtrationFilter
  8. customdry

出典と根拠

ORDレコード
ord-afac6f28e1fe4dd2a63e9071f55b752c
出典データセット
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05977139

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