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

Bromotrichloromethane → Methyl {2-{4-[(1H-Benzimidazol-1-yl)methyl]phenyl}-1,3-oxazol-4-yl}carboxylate

HRID 1716823
ノート
印刷プレビュー

反応式

HRID 1716823 の反応式
[N:1]1([CH2:10][C:11]2[CH:26]=[CH:25][C:14]([C:15]([NH:17][C@H:18]([C:21]([O:23][CH3:24])=[O:22])[CH2:19][OH:20])=O)=[CH:13][CH:12]=2)[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1.CC[N+](S(N=C(OC)[O-])(=O)=O)(CC)CC.BrC(Cl)(Cl)Cl.C1CCN2C(=NCCC2)CC1>C1COCC1.C(Cl)Cl>[N:1]1([CH2:10][C:11]2[CH:26]=[CH:25][C:14]([C:15]3[O:20][CH:19]=[C:18]([C:21]([O:23][CH3:24])=[O:22])[N:17]=3)=[CH:13][CH:12]=2)[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6383BromotrichloromethaneHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 2724994Methyl N-(triethylammoniosulfonyl)carbamateHCID 68666178HCID 68666178、化合物

生成物 1

HCID 57550219Methyl {2-{4-[(1H-Benzimidazol-1-yl)methyl]phenyl}-1,3-oxazol-4-yl}carboxylate収率 52%

試薬・触媒・溶媒 2

HCID 6344
Dichloromethane
溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

A stirred solution of methyl N-{4-[(1H-benzimidazol-1-yl)methyl]benzoyl}-serinate (2.8 g, 7.93 mmol) in THF is treated with Burgess Reagent (2.26 g, 9.45 mmol) and activated 4 Å molecular sieves (1 g), stirred at 60° C. for 2 h, cooled to room temperature and concentrated under reduced pressure. A solution of the resultant residue (0.1 g, 0.29 mmol) in CH2Cl2 is cooled to 0° C., treated with bromo trichloromethane (0.06 g, 0.33 mmol) and DBU (0.05 g, 0.33 mmol), stirred at room temperature overnight and concentrated under reduced pressure. The resultant residue is purified by column chromatography (silica, CH3OH/CHCl3 0→5%) to give the title product in 52% yield, identified by NMR and mass spectral analyses. 1H NMR (400 MHz, DMSO-d6): 8.28 (s, 1H); 8.08 (d, J=8 Hz, 2H); 8.00 (m, 1H); 7.85 (d, J=8 Hz, 2H); 7.30 (m, 5H); 5.43 (s, 2H); 3.95 (s, 3H). LCMS (ESI+) 334 (MH+).

後処理

  1. temperaturecooled to room temperature
  2. concentrationconcentrated under reduced pressure
  3. stirringstirred at room temperature overnight
  4. concentrationconcentrated under reduced pressure
  5. customThe resultant residue is purified by column chromatography (silica, CH3OH/CHCl3 0→5%)

出典と根拠

ORDレコード
ord-b66fb8fcd3a141fca1f234ca61375897
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07803825B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート