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

Benzyl Bromide → HCID 68746130、化合物

HRID 333324
ノート
印刷プレビュー

反応式

HRID 333324 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH:9]([CH2:13][NH:14][C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[C:10]([OH:12])=[O:11])=[CH:4][CH:3]=1.C([O-])([O-])=O.[K+].[K+].[CH:28]1[CH:33]=[CH:32][C:31]([CH2:34]Br)=[CH:30][CH:29]=1>CN(C=O)C.[Cl-].[Na+].O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][CH:9]([CH2:13][NH:14][C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[C:10]([O:12][CH2:34][C:31]2[CH:32]=[CH:33][CH:28]=[CH:29][CH:30]=2)=[O:11])=[CH:6][CH:7]=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 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 448910052-[(4-Bromophenyl)methyl]-3-[(tert-butoxycarbonyl)amino]propanoic acid

生成物 1

HCID 68746130HCID 68746130、化合物収率 7.1%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 57417360
Sodium chloride; water
溶媒

実験手順

A suspension of 3-(4-bromo-phenyl)-2-(tert-butoxycarbonylamino-methyl)-propionic acid (496 mg, 1.385 mmol), K2CO3 (383 mg, 2.77 mmol) and BnBr (0.493 ml, 4.15 mmol) in DMF (3 ml) was allowed to stir under nitrogen for 60 hours. The reaction mixture was cooled, and brine was added. The product was extracted with EtOAc, washed with brine, dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel (eluent: heptane/EtOAc=100:0 to 50:50) and then purified by RP-HPLC (XBridge Prep Phenyl OBD, H2O (0.1% NH4OH)/CH3CN) to give benzyl 2-(4-bromobenzyl)-3-(tert-butoxycarbonylamino)propanoate (44 mg); Retention time=1.67 minutes (condition B); MS (ES+)=348.0 (m-Boc+2).

後処理

  1. temperatureThe reaction mixture was cooled
  2. extractionThe product was extracted with EtOAc
  3. washwashed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by flash column chromatography on silica gel (eluent: heptane/EtOAc=100:0 to 50:50)
  8. custompurified by RP-HPLC (XBridge Prep Phenyl OBD, H2O (0.1% NH4OH)/CH3CN)

出典と根拠

ORDレコード
ord-961a8c8010f9448a8efc1f7f2f70ed13
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08877815B2

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