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

Water → ethyl(2E)-3-(2,1-benzisothiazol-4-yl)acrylate

HRID 1639851
ノート
印刷プレビュー

反応式

HRID 1639851 の反応式
[H-].[Na+].C(OP([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])(OCC)=O)C.[N:17]1[S:18][CH:19]=[C:20]2[C:25]([CH:26]=O)=[CH:24][CH:23]=[CH:22][C:21]=12.O>O1CCCC1>[N:17]1[S:18][CH:19]=[C:20]2[C:25](/[CH:26]=[CH:11]/[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:24][CH:23]=[CH:22][C:21]=12
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 4

HCID 962WaterHCID 13345Triethyl phosphonoacetateHCID 24758Sodium hydrideHCID 593346042,1-Benzisothiazole-4-carboxaldehyde

生成物 1

HCID 66720661ethyl(2E)-3-(2,1-benzisothiazol-4-yl)acrylate収率 380.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒
3 回

実験手順

Under nitrogen atmosphere, to a suspension of sodium hydride (60%, 1.16 g, 26.6 mmol) in tetrahydrofuran (30 mL) was added a solution of ethyl diethylphosphonoacetate (4.83 mL, 5.41 mmol) in tetrahydrofuran (10 mL) at 0° C., and the mixture was stirred for 20 min. To the reaction mixture was added a solution of 2,1-benzisothiazole-4-carbaldehyde (3.94 g, 24.1 mmol) in tetrahydrofuran (8.3 mL), and the mixture was warmed to room temperature over 4 hr. Water was added and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane=20/80) to give the title compound (4.80 g, yield 85%).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane=20/80)

出典と根拠

ORDレコード
ord-f420c0e651b540bea9a8013e119a4210
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08110585B2

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