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

Sodium Bicarbonate → (R)-1-[1-(4-Chloro-phenyl)-cyclobutanecarbonyl]-piperidine-3-carboxylic acid ethyl ester

HRID 1160354
ノート
印刷プレビュー

反応式

HRID 1160354 の反応式
C([C@@H]([C@H](C(O)=O)O)O)(O)=O.[NH:11]1[CH2:21][CH2:20][CH2:19][C@@H:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:12]1.C(=O)(O)[O-].[Na+].[Cl:27][C:28]1[CH:33]=[CH:32][C:31]([C:34]2([C:38](Cl)=[O:39])[CH2:37][CH2:36][CH2:35]2)=[CH:30][CH:29]=1>ClCCl>[CH2:17]([O:16][C:14]([C@@H:13]1[CH2:19][CH2:20][CH2:21][N:11]([C:38]([C:34]2([C:31]3[CH:30]=[CH:29][C:28]([Cl:27])=[CH:33][CH:32]=3)[CH2:35][CH2:36][CH2:37]2)=[O:39])[CH2:12]1)=[O:15])[CH3:18]
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 516892Sodium BicarbonateHCID 130833731-(4-Chlorophenyl)cyclobutane-1-carbonyl chlorideHCID 14183616Ethyl (R)-Nipecotate L-Tartrate

生成物 1

HCID 58737402(R)-1-[1-(4-Chloro-phenyl)-cyclobutanecarbonyl]-piperidine-3-carboxylic acid ethyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Ethyl (R)-nipecotate L-tartrate (15.0 g, 48.8 mmol) was added to a stirred mixture of dichloromethane and saturated sodium bicarbonate solution (100 mL each) at 0° C. After 10 min 1-(4-chloro-phenyl)-cyclobutanecarbonyl chloride (11.13 g, 48.8 mmol) was slowly added at 0° C. The reaction was then allowed to stir for 2 h at room temperature. The organic layer was separated and the aqueous layer was washed once with dichloromethane (100 mL). The organic material was combined and washed once with water (100 mL), dried over anhydrous sodium sulfate, filtered and concentrated by rotary evaporation. The residue was purified by chromatography on silica gel, eluting with hexane/ethyl acetate (2:1) to give 9.2 g of the amidester as a thick clear gum; C19H24ClNO3, LRMS (m/z)=350 (MH+).

後処理

  1. customThe organic layer was separated
  2. washthe aqueous layer was washed once with dichloromethane (100 mL)
  3. washwashed once with water (100 mL)
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated by rotary evaporation
  7. customThe residue was purified by chromatography on silica gel
  8. washeluting with hexane/ethyl acetate (2:1)
  9. customto give 9.2 g of the amidester as a thick clear gum

出典と根拠

ORDレコード
ord-83d10848c32c4455b3a500582b5cea2a
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07816375B2

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