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

1-(2-Methoxyphenyl)piperazine → HCID 19752298、化合物

HRID 1885310
ノート
印刷プレビュー

反応式

HRID 1885310 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][NH:5][C:6]([C:8]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[S:10][N:9]=1)=[O:7].[CH3:17][O:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[N:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN1CCCC1=O>[ClH:1].[ClH:1].[CH3:17][O:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[N:25]1[CH2:30][CH2:29][N:28]([CH2:2][CH2:3][CH2:4][NH:5][C:6]([C:8]2[C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=3[S:10][N:9]=2)=[O:7])[CH2:27][CH2:26]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

6

反応物 4

HCID 13461-(2-Methoxyphenyl)piperazineHCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 10332575HCID 10332575、化合物

生成物 1

HCID 19752298HCID 19752298、化合物収率 53.2%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
180 °C

実験手順

A mixture of N-(3-chloropropyl)-1,2-benzisothiazole-3-carboxamide (4.2 g), 1-(2-methoxyphenyl)piperazine (3.3 g), potassium carbonate (4.55 g), and sodium iodide (100 mg) in dry N-methylpyrrolidinone (150 ml) was heated to 180° C., with stirring, under nitrogen. After 24 hr, the reaction mixture was allowed to cool to room temperature and partitioned between ether/water. The organic phase was dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated in vacuo. The residue was chromatographed on silica using ether as the eluent. The appropriate fractions were collected and evaporated. The residue was taken up in ether and hydrogen chloride in ether was added. Recrystallization of the precipitate from methanol/dichloromethane/ether provided 2.12 g (26.6%) of product, mp 191°-194° C.

後処理

  1. temperatureto cool to room temperature
  2. custompartitioned between ether/water
  3. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated in vacuo
  6. customThe residue was chromatographed on silica
  7. customThe appropriate fractions were collected
  8. customevaporated
  9. additionhydrogen chloride in ether was added
  10. customRecrystallization of the precipitate from methanol/dichloromethane/ether

出典と根拠

ORDレコード
ord-b2ad1499fd6a4ebbaecf836c7adab0d9
出典データセット
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05143923

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