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

Formic Acid → HCID 76652336、化合物

HRID 1434903
ノート
印刷プレビュー

反応式

HRID 1434903 の反応式
[CH:1](O)=[O:2].C(OC(=O)C)(=O)C.[CH2:11]([CH:18]1[CH2:22][O:21][C:20](=[O:23])[N:19]1[C:24](=[O:41])[CH:25]([CH2:35][CH:36]1[CH2:40][CH2:39][CH2:38][CH2:37]1)[CH2:26][NH:27][O:28][CH:29]1[CH2:34][CH2:33][CH2:32][CH2:31][O:30]1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.CCN(CC)CC>C(Cl)Cl>[CH2:11]([CH:18]1[CH2:22][O:21][C:20](=[O:23])[N:19]1[C:24](=[O:41])[CH:25]([CH2:35][CH:36]1[CH2:37][CH2:38][CH2:39][CH2:40]1)[CH2:26][N:27]([O:28][CH:29]1[CH2:34][CH2:33][CH2:32][CH2:31][O:30]1)[CH:1]=[O:2])[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1
参加物反応条件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 284Formic AcidHCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 76652338HCID 76652338、化合物

生成物 1

HCID 76652336HCID 76652336、化合物収率 87.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
50 °C

実験手順

A mixture of formic acid (45.0 mL, 1193 mmol) and acetic anhydride (90.0 mL, 952 mmol) is stirred at 50° C. for one hour under nitrogen. A second flask is charged with 4-benzyl-3-[2-cyclopentylmethyl-3-(tetrahydro-pyran-2-yloxyamino)-propionyl]-oxazolidin-2-one (21.62 g, 50.2 mmol), Et3N (170.0 mL, 1220 mmol), and anhydrous DCM (450 mL). This second mixture is cooled to 4° C. under nitrogen, and the mixed acid solution is slowly added to the second flask, while maintaining 10° C. The combined mixture is stirred for 30 minutes at 10° C., quenched with saturated, washed with aqueous NaHCO3 solution, and extracted with DCM. The DCM layers are combined, dried over Na2SO4, and concentrated. The crude product is purified by flash chromatography (SiO2, 50% EtOAc in hexane), which gives N-[3-(4-benzyl-2-oxo-oxazolidin-3-yl)-2-cyclopentylmethyl-3-oxo-propyl]-N-(tetrahydro-pyran-2-yloxy)-formamide (20.10 g, 87% yield) as an oil.

後処理

  1. temperatureThis second mixture is cooled to 4° C. under nitrogen
  2. additionthe mixed acid solution is slowly added to the second flask
  3. temperaturewhile maintaining 10° C
  4. stirringThe combined mixture is stirred for 30 minutes at 10° C.
  5. customquenched with saturated,
  6. washwashed with aqueous NaHCO3 solution
  7. extractionextracted with DCM
  8. dry with materialdried over Na2SO4
  9. concentrationconcentrated
  10. customThe crude product is purified by flash chromatography (SiO2, 50% EtOAc in hexane), which

出典と根拠

ORDレコード
ord-f665df997e9a45c094273a88a406fa7f
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07615635B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート