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 → HCID 178482132、化合物

HRID 504161
ノート
印刷プレビュー

反応式

HRID 504161 の反応式
C1CN([P+](ON2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.C(N(CC)CC)C.[F:41][C:42]([F:62])([F:61])[C:43]1[CH:44]=[C:45]([S:49]([N:52]2[CH2:57][CH2:56][CH2:55][CH2:54][C@H:53]2[C:58]([OH:60])=O)(=[O:51])=[O:50])[CH:46]=[CH:47][CH:48]=1.[NH2:63][C@@H:64]([CH2:75][C:76]1[CH:81]=[CH:80][CH:79]=[CH:78][CH:77]=1)/[CH:65]=[N:66]/[C:67]1[C:68]([NH:73][CH3:74])=[CH:69][CH:70]=[CH:71][CH:72]=1>C(Cl)Cl>[CH2:75]([C@H:64]([NH:63][C:58]([C@@H:53]1[CH2:54][CH2:55][CH2:56][CH2:57][N:52]1[S:49]([C:45]1[CH:46]=[CH:47][CH:48]=[C:43]([C:42]([F:41])([F:61])[F:62])[CH:44]=1)(=[O:50])=[O:51])=[O:60])/[CH:65]=[N:66]/[C:67]1[CH:72]=[CH:71][CH:70]=[CH:69][C:68]=1[NH:73][CH3:74])[C:76]1[CH:77]=[CH:78][CH:79]=[CH:80][CH:81]=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 8471TriethylamineHCID 2724699PyBOPHCID 59428653HCID 59428653、化合物HCID 178482134HCID 178482134、化合物

生成物 1

HCID 178482132HCID 178482132、化合物収率 64%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒
3 回

実験手順

PyBOP (0.11 g, 0.22 mmoles) and triethylamine (0.076 mL, 0.55 mmoles) were added to a room temperature solution of (S)-1-(3-trifluoromethyl-benzenesulfonyl)-piperidine-2-carboxylic acid (0.074 g, 0.22 mmol) in CH2Cl2 (5 mL). After stirring at room temperature for 20 min, a solution of N-[(S)-2-amino-3-phenyl-prop-(E)-ylidene]-N′-methyl-benzene-1,2-diamine (0.052 g, 0.22 mmoles) in CH2Cl2 (5 mL) was added, and the resulting mixture was stirred at room temperature for 16 h. The reaction mixture was diluted with CH2Cl2 (100 mL) and washed with saturated aqueous NaHCO3 (100 mL) and brine (100 mL). The organic layer was dried (MgSO4) and concentrated in vacuo to give a yellow oil. Purification of the residue by flash chromatography on silica gel, eluting with 10-50% EtOAc/heptane afforded 0.078 g (64%) of the title compound as a colorless powder: ES+ LC/MS m/e 557 (M+H), RT=2.92 min; 1H NMR CDCl3: δ9.99 (bd s, 1), 8.05 (s, 1), 7.94 (d, 1, J=8.0 Hz), 7.83 (d, 1, J=7.9 Hz), 7.62 (t, 1, J=7.9 Hz), 7.23-7.56 (m, 8), 7.00 (d, 1, J=7.5 Hz), 5.45 (m, 1), 4.40 (bd s, 1), 3.72 (dd, 1, J=14.5, 5.1 Hz), 3.54 (d, 1, J=14.1 Hz), 3.44 (dd, 1, J=14.5, 10.8 Hz), 2.13-2.26 (m, 2), 1.37 (m, 1), 1.22 (m, 1), 0.92-1.10 (m, 4).

後処理

  1. stirringthe resulting mixture was stirred at room temperature for 16 h
  2. washwashed with saturated aqueous NaHCO3 (100 mL) and brine (100 mL)
  3. dry with materialThe organic layer was dried (MgSO4)
  4. concentrationconcentrated in vacuo
  5. customto give a yellow oil
  6. customPurification of the residue by flash chromatography on silica gel
  7. washeluting with 10-50% EtOAc/heptane

出典と根拠

ORDレコード
ord-ecb3af95d73c4c33a1ad5122eb7660c4
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07777042B2

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