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 → HCID 89668315、化合物

HRID 1482248
ノート
印刷プレビュー

反応式

HRID 1482248 の反応式
C([O:5][C:6]([NH:8][C@H:9]([C:29](=[O:36])[N:30]1[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]1)[CH2:10][C:11]1[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][C:22]([O:24]C(C)(C)C)=[O:23])=[CH:13][CH:12]=1)=[O:7])(C)(C)C.FC(F)(F)C(O)=O.C(=O)([O-])[O-].[Na+].[Na+].[CH:50]1[C:62]2[CH:61]([CH2:63]OC(ON3C(=O)CCC3=O)=O)[C:60]3[C:55](=[CH:56][CH:57]=[CH:58][CH:59]=3)[C:54]=2[CH:53]=[CH:52][CH:51]=1>C(Cl)Cl>[CH:50]1[C:62]2[CH:61]([CH2:63][O:5][C:6]([NH:8][C@H:9]([C:29](=[O:36])[N:30]3[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35]3)[CH2:10][C:11]3[CH:12]=[CH:13][C:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][C:22]([OH:24])=[O:23])=[CH:15][CH:16]=3)=[O:7])[C:60]3[C:55](=[CH:56][CH:57]=[CH:58][CH:59]=3)[C:54]=2[CH:53]=[CH:52][CH:51]=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 6422Trifluoroacetic acidHCID 10340Sodium CarbonateHCID 134122N-(9-Fluorenylmethoxycarbonyloxy)succinimideHCID 89668519HCID 89668519、化合物

生成物 1

HCID 89668315HCID 89668315、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

実験手順

tert-Butyl (S)-6-(4-(2-((tert-butoxycarbonyl)amino)-3-oxo-3-(piperidin-1-yl)propyl)phenyl)hexanoate (Compound SP426) (5.65 g, 11.24 mmol) was dissolved in DCM (30.0 ml), trifluoroacetic acid (15.0 ml, 195 mmol) was added and the mixture was stirred for 30 minutes at room temperature, after which the reaction solution was concentrated under reduced pressure. The resulting residue was dissolved in dioxane (40 ml) and a 10% aqueous sodium carbonate solution (80 ml), N-(9-fluorenylmethoxycarbonyloxy)-succinimide (3.68 g, 10.90 mmol) was added and the mixture was stirred at room temperature for 1 hour. The reaction solution was washed with diethyl ether, made acidic by adding a 5 N aqueous HCl solution and then extracted with ethyl acetate. The ethyl acetate layer was dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to afford the title compound SP427 (6.39 g, 100%).

後処理

  1. concentrationafter which the reaction solution was concentrated under reduced pressure
  2. dissolutionThe resulting residue was dissolved in dioxane (40 ml)
  3. stirringthe mixture was stirred at room temperature for 1 hour
  4. washThe reaction solution was washed with diethyl ether
  5. additionby adding a 5 N aqueous HCl solution
  6. extractionextracted with ethyl acetate
  7. dry with materialThe ethyl acetate layer was dried over anhydrous Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-8012aa0412e44209a48b6fbec1eb7c7f
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09409952B2

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