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 → 4-benzenesulfinyl-N-{2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-benzamide

HRID 1177844
ノート
印刷プレビュー

反応式

HRID 1177844 の反応式
CCN(C(C)C)C(C)C.[C:10]1([S:16]([C:18]2[CH:26]=[CH:25][C:21]([C:22]([OH:24])=O)=[CH:20][CH:19]=2)=[O:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.[NH2:48][CH2:49][C:50]([N:52]1[CH2:57][CH2:56][N:55]([C:58](=[O:69])[C:59]2[CH:64]=[CH:63][CH:62]=[CH:61][C:60]=2[C:65]([F:68])([F:67])[F:66])[CH2:54][CH2:53]1)=[O:51].C(O)(C(F)(F)F)=O>CN(C=O)C.O>[C:10]1([S:16]([C:18]2[CH:19]=[CH:20][C:21]([C:22]([NH:48][CH2:49][C:50](=[O:51])[N:52]3[CH2:53][CH2:54][N:55]([C:58](=[O:69])[C:59]4[CH:64]=[CH:63][CH:62]=[CH:61][C:60]=4[C:65]([F:66])([F:68])[F:67])[CH2:56][CH2:57]3)=[O:24])=[CH:25][CH:26]=2)=[O:17])[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 6422Trifluoroacetic acidHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 3438114-Benzenesulfinyl-benzoic acidHCID 595596292-Amino-1-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethanone

生成物 1

HCID 25167126
4-benzenesulfinyl-N-{2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-benzamide
収率 51%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

DIPEA (0.084 mL, 0.49 mmol) was added drop wise to 4-benzenesulfinyl-benzoic acid (48 mg, 0.19 mmol) in DMF (4 mL). EDCI (78 mg, 0.41 mmol) and HOBT 26 mg, 0.19 mmol) were added consecutively and 2-amino-1-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethanone in its TFA salt form (70 mg, 0.16 mmol) was added after a further 10 mins. The resulting mixture was allowed to stir at room temperature overnight. Water was then added and the product was extracted with EtOAc and washed with brine. The organic phase was dried over Na2SO4 and concentrated under reduced pressure to afford a crude product. Purification by column chromatography (using silica gel with a mesh size of 60-120 and 100% EtOAc as eluent) afforded 45 mg (51% yield) of 4-benzenesulfinyl-N-{2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-benzamide. LC-MS purity: 91.93%. 1H NMR (DMSO-D6): δ 8.7 (t, 1H), 8 (m, 3H), 7.8 (m, 6H), 7.5 (m, 3H), 7.2 (m, 1H), 4.2 (d, 2H), 3.6 (m, 6H), 3.1 (m, 2H).

後処理

  1. extractionthe product was extracted with EtOAc
  2. washwashed with brine
  3. dry with materialThe organic phase was dried over Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. customto afford a crude product
  6. customPurification by column chromatography (

出典と根拠

ORDレコード
ord-2578c01d2e5243ff8ae15ab14638c5d6
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07842696B2

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