Methyl iodide → 6-Amino-4-methyl-2H-1,4-benzothiazin-3(4H)-one

HRID 9720

反応式

HRID 9720 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[S:10][CH2:9][C:8](=[O:11])[NH:7][C:6]=2[CH:12]=1.[H-].[Na+].[CH3:15]I.[Cl-].[NH4+]>CN(C=O)C>[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[S:10][CH2:9][C:8](=[O:11])[N:7]([CH3:15])[C:6]=2[CH:12]=1

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 6869016-amino-3,4-dihydro-2H-1,4-benzothiazin-3-one

生成物 1

HCID 219881476-Amino-4-methyl-2H-1,4-benzothiazin-3(4H)-one収率 63.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4.5 g 6-Amino-4H-benzo[1,4]thiazin-3-one in 50 ml DMF was treated in portions with 0.695 g 95% sodium hydride at room temperature. After 30 min, 3.548 g methyl iodide were added dropwise at 0° C. and stirring was continued for another 30 min. The mixture was poured into ice and ammonium chloride solution and extracted with CH2Cl2. Chromatography on silica yielded 3.1 g crude product, which was further purified by trituration with diethyl ether.

後処理

  1. waitwas continued for another 30 min
  2. extractionextracted with CH2Cl2

出典と根拠

ORDレコード
ord-ae7541c76b774e8fa0cc87517c966110
出典データセット
uspto-grants-2006_08
特許番号
US07091345B2

関連ノート

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