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

Potassium Carbonate → Tert-butyl 2-ethynyl-6-methoxyphenylcarbamate

HRID 1095692
ノート
印刷プレビュー

反応式

HRID 1095692 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]#[C:10][Si](C)(C)C)[C:4]=1[NH:15][C:16](=[O:22])[O:17][C:18]([CH3:21])([CH3:20])[CH3:19].C([O-])([O-])=O.[K+].[K+]>CO>[C:9]([C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[C:4]=1[NH:15][C:16](=[O:22])[O:17][C:18]([CH3:20])([CH3:19])[CH3:21])#[CH:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 10829462Tert-butyl 2-methoxy-6-((trimethylsilyl)ethynyl)phenylcarbamate

生成物 1

HCID 86638604Tert-butyl 2-ethynyl-6-methoxyphenylcarbamate収率 62%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To tert-butyl 2-methoxy-6-((trimethylsilyl)ethynyl)phenylcarbamate (4.21 g, 13.2 mmol) in MeOH (30 mL) was added K2CO3 (9.11 g, 65.9 mmol). The reaction was stirred for 30 minutes, then filtered and washed with DCM (50 mL). The combined organic layers were concentrated and diluted with DCM (20 mL), filtered, washed a second time with DCM (50 mL), then concentrated. The residue was purified by flash chromatography through a pad of silica gel with 10:1 Hexane/EtOAc (500 mL), affording the desired product (62%).

後処理

  1. filtrationfiltered
  2. washwashed with DCM (50 mL)
  3. concentrationThe combined organic layers were concentrated
  4. additiondiluted with DCM (20 mL)
  5. filtrationfiltered
  6. washwashed a second time with DCM (50 mL)
  7. concentrationconcentrated
  8. customThe residue was purified by flash chromatography through a pad of silica gel with 10:1 Hexane/EtOAc (500 mL)

出典と根拠

ORDレコード
ord-6895bced2787464cb18398dad8c1202a
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08138181B2

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