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

Allyl bromide → HCID 19737997、化合物

HRID 2255506
ノート
印刷プレビュー

反応式

HRID 2255506 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+].[CH2:15](Br)[CH:16]=[CH2:17]>CN(C=O)C>[CH2:17]([N:4]1[CH2:3][CH:2]([OH:1])[C:7]2[CH:8]=[CH:9][S:10][C:6]=2[S:5]1(=[O:12])=[O:11])[CH:16]=[CH2:15]
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 7841Allyl bromideHCID 24758Sodium hydrideHCID 229019424-Hydroxy-3,4-dihydro-2H-thieno[3,2-e][1,2]thiazine 1,1-dioxide

生成物 1

HCID 19737997HCID 19737997、化合物収率 88%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
-10 °C

実験手順

The product from Step C of Example 2 (4.0 g, 19.5 mmol) was dissolved in anhydrous DMF (70 mL) cooled to -10° C. and sodium hydride (21.5 mmol) was added. After stirring for five minutes allyl bromide (2.53 mL, 29.25 mmol) was added and this mixture stirred for 2 h at 0° C. The reaction mixture was poured onto ice water (100 mL) and this solution was extracted with ethyl acetate. The combined extracts were washed with brine, dried (MgSO4) and evaporated to give a crude product which was purified by column chromatography (silica, methylene chloride:methanol, 20:1) to provide the desired product (4.2 g, 88%) as a syrup.

後処理

  1. additionwas added
  2. additionThe reaction mixture was poured onto ice water (100 mL)
  3. extractionthis solution was extracted with ethyl acetate
  4. washThe combined extracts were washed with brine
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customto give a crude product which
  8. customwas purified by column chromatography (silica, methylene chloride:methanol, 20:1)

出典と根拠

ORDレコード
ord-787f612a7ee14d269243e2299d5df1d9
出典データセット
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05240923

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