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

Triethylamine → 4-(3-tert-Butoxycarbonylaminopyrrolidin-1-yl)-2,5-difluorobenzoic acid ethyl ester

HRID 10287
ノート
印刷プレビュー

反応式

HRID 10287 の反応式
[CH2:1]([O:3][C:4](=[O:14])[C:5]1[CH:10]=[C:9]([F:11])[C:8](F)=[CH:7][C:6]=1[F:13])[CH3:2].C(N(CC)CC)C.[C:22]([O:26][C:27](=[O:34])[NH:28][CH:29]1[CH2:33][CH2:32][NH:31][CH2:30]1)([CH3:25])([CH3:24])[CH3:23]>C(#N)C.C(OCC)(=O)C>[CH2:1]([O:3][C:4](=[O:14])[C:5]1[CH:10]=[C:9]([F:11])[C:8]([N:31]2[CH2:32][CH2:33][CH:29]([NH:28][C:27]([O:26][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:34])[CH2:30]2)=[CH:7][C:6]=1[F:13])[CH3:2]
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 3

HCID 8471TriethylamineHCID 2757234tert-butyl N-(pyrrolidin-3-yl)carbamateHCID 2774397Benzoic acid, 2,4,5-trifluoro-, ethyl ester

生成物 1

HCID 690751024-(3-tert-Butoxycarbonylaminopyrrolidin-1-yl)-2,5-difluorobenzoic acid ethyl ester

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

To a solution of 2,4,5-trifluorobenzoic acid ethyl ester (Example 1e, 14.8 g, 72.4 mmol) in acetonitrile (225 mL) is added triethylamine (65 mL, 466 mmol) and pyrrolidin-3-ylcarbamic acid tert-butyl ester (16.07 g, 86.2 mmol). After 45 hours, the reaction mixture is diluted with ethyl acetate and washed with saturated NaHCO3, water, and brine. The organic layer is dried over MgSO4, filtered, and the filtrate is concentrated to afford an oil. The resulting residue is purified by flash chromatography (1:5 ethyl acetate/hexanes) to afford the title compound. MS (ES, M+1) m/z 371, mp 98–100° C.

後処理

  1. washwashed with saturated NaHCO3, water, and brine
  2. dry with materialThe organic layer is dried over MgSO4
  3. filtrationfiltered
  4. concentrationthe filtrate is concentrated
  5. customto afford an oil
  6. customThe resulting residue is purified by flash chromatography (1:5 ethyl acetate/hexanes)

出典と根拠

ORDレコード
ord-0a282666be1a4e63bfa975c0f623bbd3
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07094780B1

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