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Sodium Iodide → HCID 19752325、化合物

HRID 483431
ノート
印刷プレビュー

反応式

HRID 483431 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].Cl.[Cl:18][C:19]1[CH:33]=[CH:32][C:22]2[C:23]([N:26]3[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]3)=[N:24][O:25][C:21]=2[CH:20]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN1CCCC1=O>[ClH:1].[Cl:18][C:19]1[CH:33]=[CH:32][C:22]2[C:23]([N:26]3[CH2:27][CH2:28][CH:29]([CH2:2][CH2:3][CH2:4][NH:5][C:6]([C:8]4[C:12]5[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=5[S:10][N:9]=4)=[O:7])[CH2:30][CH2:31]3)=[N:24][O:25][C:21]=2[CH:20]=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 5238Sodium IodideHCID 11430Potassium CarbonateHCID 10332575HCID 10332575、化合物HCID 19752293HCID 19752293、化合物

生成物 1

HCID 19752325HCID 19752325、化合物収率 29.8%

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 (5.0 g), 1-(6-chloro-1,2-benzisoxazol-3-yl)piperidine hydrochloride (5.40 g), potassium carbonate (5.40 g), and sodium iodide (100 mg) in dry N-methylpyrrolidinone (100 ml), was heated to 180° C., with stirring, under nitrogen. After 36 hr, the reaction mixture was allowed to cool to room temperature and partitioned between ethyl acetate/water. The organic phase was washed with water, dried over anhydrous magnesium sulfate, filtered, and the filtrate concentrated in vacuo. The residue was chromatographed on silica using ethyl acetate as the eluent. The appropriate fractions were collected and concentrated. The filtrate was treated with hydrogen chloride in ether. The salt was recrystallized from methanol/dichloromethane/ether to provide 2.87 g (29.4%) of product, mp 221°-223° C.

後処理

  1. temperatureto cool to room temperature
  2. custompartitioned between ethyl acetate/water
  3. washThe organic phase was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationthe filtrate concentrated in vacuo
  7. customThe residue was chromatographed on silica
  8. customThe appropriate fractions were collected
  9. concentrationconcentrated
  10. additionThe filtrate was treated with hydrogen chloride in ether
  11. customThe salt was recrystallized from methanol/dichloromethane/ether

出典と根拠

ORDレコード
ord-e703a74e4a4642f499d42c8c68ed3f15
出典データセット
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05225412

反応ノート

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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