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

Trifluoroacetic acid → (2-Ethylthiazol-4-yl)(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone trifluoroacetate

HRID 1255314
ノート
印刷プレビュー

反応式

HRID 1255314 の反応式
[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[CH2:8]([C:10]1[S:11][CH:12]=[C:13]([C:15]([N:17]2[CH2:22][C:21]3([CH2:27][CH2:26][N:25](C(OC(C)(C)C)=O)[CH2:24][CH2:23]3)[O:20][CH2:19][CH2:18]2)=[O:16])[N:14]=1)[CH3:9]>ClCCl.C1(C)C=CC=CC=1>[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[CH2:8]([C:10]1[S:11][CH:12]=[C:13]([C:15]([N:17]2[CH2:22][C:21]3([CH2:27][CH2:26][NH:25][CH2:24][CH2:23]3)[O:20][CH2:19][CH2:18]2)=[O:16])[N:14]=1)[CH3:9]
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 2

HCID 6422Trifluoroacetic acidHCID 58168458Tert-butyl 4-(2-ethylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecane-9-carboxylate

生成物 1

HCID 66964094(2-Ethylthiazol-4-yl)(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone trifluoroacetate

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒

実験手順

Trifluoroacetic acid (20 mL) was added to a solution of tert-butyl 4-(2-ethylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecane-9-carboxylate [Example 26, step a] (24 g) in dichloromethane (100 mL) and the mixture stirred at ambient temperature for 18 hours. The reaction mixture was diluted with toluene (50 mL) and concentrated in vacuo. The residue was dissolved in dichloromethane (50 mL), TFA (50 mL) was added and the mixture was stirred for 4 hours. The mixture was diluted with toluene (50 mL), concentrated in vacuo, the residue triturated with ether and the precipitated solid collected by filtration and dried to afford the subtitled compound as a white solid. Yield 28 g.

後処理

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue was dissolved in dichloromethane (50 mL)
  3. additionTFA (50 mL) was added
  4. stirringthe mixture was stirred for 4 hours
  5. additionThe mixture was diluted with toluene (50 mL)
  6. concentrationconcentrated in vacuo
  7. customthe residue triturated with ether
  8. filtrationthe precipitated solid collected by filtration
  9. customdried

出典と根拠

ORDレコード
ord-3e553ab8c2dd4696a48ded35e5d82b60
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08455483B2

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