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

Dimethylformamide → HCID 21193267、化合物

HRID 443275
ノート
印刷プレビュー

反応式

HRID 443275 の反応式
C(OC([N:8]1[CH2:16][CH2:15][C:11]([CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[CH:19]=2)([C:12](O)=[O:13])[CH2:10][CH2:9]1)=O)(C)(C)C.Cl.CN(C)[CH2:28][CH2:29][CH2:30]N=C=NCC.[OH2:37].ON1C2C=CC=CC=2N=N1.[Cl-].[NH4+:49].[CH:50](N(C(C)C)CC)(C)C.CN(C)[CH:61]=[O:62]>>[C:29]([O:37][C:61]([NH:49][C:12](=[O:13])[C:11]1([CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[CH:19]=2)[CH2:15][CH2:16][NH:8][CH2:9][CH2:10]1)=[O:62])([CH3:30])([CH3:50])[CH3:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 6

HCID 6228DimethylformamideHCID 25517Ammonium ChlorideHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 211933671-Boc-4-(3-methylbenzyl)-4-carboxypiperidine

生成物 1

HCID 21193267
HCID 21193267、化合物

実験手順

A mixture of N-tert-butoxycarbonyl-4-(3-methylbenzyl)-isonipecotic acid (1.02 g, 3.00 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.64 g. 3.36 mmol), 1-hydroxy-benzotriazole hydrate (0.45 g, 3.31 mmol), ammonium chloride (0.33 g, 6.15 mmol), and diisopropylethylamine (1.15 mL, 6.60 mmol) in anhydrous dimethylformamide (10 ml) was stirred at room temp. overnight. The resultant solution was concentrated under vacuum and the residue was partitioned between ethyl acetate and water. The organic extracts were combined, washed with brine, dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum. The residual oil was subjected to column chromatography on silica eluting with 40% ethyl acetate in hexane. Collection and concentration of appropriate fractions provided the title product.

後処理

  1. concentrationThe resultant solution was concentrated under vacuum
  2. customthe residue was partitioned between ethyl acetate and water
  3. washwashed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum
  7. customCollection and concentration of appropriate fractions

出典と根拠

ORDレコード
ord-e525b29e10f04bd1b8ab78b2f3f0d677
出典データセット
uspto-grants-1999_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05891889

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