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

Hydrochloric Acid → HCID 45275700、化合物

HRID 1667081
ノート
印刷プレビュー

反応式

HRID 1667081 の反応式
[CH2:1]([CH:8]1[CH2:13][NH:12][CH2:11][CH2:10][N:9]1C(OC(C)(C)C)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[O:21]=[C:22]1[C:26]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH2:25][CH2:24][N:23]1[CH2:39][C:40](O)=[O:41].C(N(C(C)C)CC)(C)C.Cl>ClCCl>[CH2:1]([CH:8]1[NH:9][CH2:10][CH2:11][N:12]([C:40](=[O:41])[CH2:39][N:23]2[CH2:24][CH2:25][C:26]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[C:22]2=[O:21])[CH2:13]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 81531DiisopropylethylamineHCID 44118663tert-Butyl 2-benzylpiperazine-1-carboxylateHCID 673590132-(2-Oxo-3,3-diphenylpyrrolidin-1-yl)acetic acid

生成物 1

HCID 45275700HCID 45275700、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

実験手順

To tert-butyl 2-benzylpiperazine-1-carboxylate (0.052 g, 0.190 mmol), 2-(2-oxo-3,3-diphenylpyrrolidin-1-yl)acetic acid (Example 1C, 0.051 g, 0.173 mmol) and 2-(1H-benzo[d][1,2,3]triazol-1-yl)-1,1,3,3-tetramethylisouronium hexafluorophosphate(V) (0.069 g, 0.181 mmol) in dichloromethane (0.5 mL) was added diisopropylethylamine (0.045 mL, 0.259 mmol), and the reaction was stirred a room temperature. After stirring overnight, the reaction was concentrated, loaded onto a silica gel column (Analogix® SF15-12, Burlington, Wis.) and eluted with a gradient of 5% to 100% ethyl acetate/hexanes. To the resulting product was added HCl (2.0 Min diethyl ether, 3.57 μl, 0.117 mmol), and the reaction was stirred at room temperature overnight. The reaction was centrifuged, and the solvent was decanted away from the solid. Diethyl ether (1 mL) was added, and the suspension was sonicated to give a fine suspension. The reaction was centrifuged, the solvent was decanted and the resulting solid dried to give the title compound as the hydrochloride salt. 1H NMR (300 MHz, pyridine-d5) δ ppm 7.05-7.50 (m, 15H), 4.65-4.80 (m, 2H), 4.25-4.55 (m, 2H), 3.95-4.15 (m, 2H), 3.40-3.75 (m, 5H), 2.95-3.27 (m, 2H), 2.75-2.85 (m, 2H); MS (DCI+) m/z 454.2 (M+H)+.

後処理

  1. stirringAfter stirring overnight
  2. concentrationthe reaction was concentrated
  3. washeluted with a gradient of 5% to 100% ethyl acetate/hexanes
  4. stirringthe reaction was stirred at room temperature overnight
  5. customthe solvent was decanted away from the solid
  6. additionDiethyl ether (1 mL) was added
  7. customthe suspension was sonicated
  8. customto give a fine suspension
  9. customthe solvent was decanted
  10. customthe resulting solid dried

出典と根拠

ORDレコード
ord-2d9700144a654a12a472e733622a9bac
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08044069B2

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