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

Sodium hydride → HCID 22901897、化合物

HRID 1489816
ノート
印刷プレビュー

反応式

HRID 1489816 の反応式
[OH:1][CH:2]1[C:7]2[CH:8]=[CH:9][S:10][C:6]=2[S:5](=[O:12])(=[O:11])[NH:4][CH2:3]1.[H-].[Na+].[CH3:15][O:16][CH2:17][CH2:18][CH2:19]Br>CN(C=O)C>[OH:1][CH:2]1[C:7]2[CH:8]=[CH:9][S:10][C:6]=2[S:5](=[O:12])(=[O:11])[N:4]([CH2:19][CH2:18][CH2:17][O:16][CH3:15])[CH2:3]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

5

反応物 3

HCID 24758Sodium hydrideHCID 5245511-Bromo-3-methoxypropaneHCID 229019424-Hydroxy-3,4-dihydro-2H-thieno[3,2-e][1,2]thiazine 1,1-dioxide

生成物 1

HCID 22901897HCID 22901897、化合物収率 63%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

The product from Example 1, Step C (2.0 g, 9.74 mmol) was added to a suspension of sodium hydride (0.4 g, 10.0 mmol, of a 60% suspension in mineral oil) in DMF (30 ML) and the mixture was stirred for 1hr. then cooled to 0° C. 3-Bromopropyl methyl ether (1.5 g, 9.74 mmol) was added and the mixture was stirred overnight then quenched with water (200 mL), and extracted with ethyl acetate (4×30 mL). The extracts were combined, washed with water (100 mL), dried (MgSO4) and concentrated under reduced pressure which provided an oil which was purified by column chromatography (silica, gradient: hexane to ethyl acetate) to give 1.7 g (63%) of a clear oil which was not purified further.

後処理

  1. customthen quenched with water (200 mL)
  2. extractionextracted with ethyl acetate (4×30 mL)
  3. washwashed with water (100 mL)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated under reduced pressure which
  6. customprovided an oil which
  7. customwas purified by column chromatography (silica, gradient: hexane to ethyl acetate)

出典と根拠

ORDレコード
ord-88aa6f12fda945dd82f6513ea9e70b86
出典データセット
uspto-grants-1997_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05679670

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