2-Methylpyridine → Sodium 4-(benzothiazol-2-yl)phenylsulphamate

HRID 1636566

反応式

HRID 1636566 の反応式
N1C=CC=CC=1C.Cl[S:9]([OH:12])(=[O:11])=[O:10].[NH2:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[S:21][C:22]3[CH:28]=[CH:27][CH:26]=[CH:25][C:23]=3[N:24]=2)=[CH:16][C:15]=1I.C(=O)([O-])[O-].[Na+:34].[Na+]>>[S:21]1[C:22]2[CH:28]=[CH:27][CH:26]=[CH:25][C:23]=2[N:24]=[C:20]1[C:17]1[CH:18]=[CH:19][C:14]([NH:13][S:9](=[O:11])(=[O:10])[O-:12])=[CH:15][CH:16]=1.[Na+:34]

参加物

5

反応物 4

HCID 79752-MethylpyridineHCID 10340Sodium CarbonateHCID 24638Chlorosulfonic acidHCID 384526Benzenamine, 4-(2-benzothiazolyl)-2-iodo-

生成物 1

HCID 23717892Sodium 4-(benzothiazol-2-yl)phenylsulphamate

反応条件

温度
50 °C

実験手順

To anhydrous 2-picoline (1.05 g, 11 mmol) was slowly added dropwise chlorsulphonic acid (0.26 g, 2.21 mmol) below 10° C. then 2-(4'-amino-3'-iodophenyl)benzothiazole (0.5 g, 2.21 mmol). The mixture was heated to 50° C. with stirring for 1 hour. After leaving to stand for 2 hours at room temperature, 6 ml of 10% aqueous sodium carbonate was added. The resulting mixture was stirred for 40 minutes at room temperature and concentrated under reduced pressure. The precipitate was filtered off, washed carefully with cold water and treated with hot chlorform. Golden crystals were afforded (0.62 g, 85.5%), m.p. 288-290° C.

後処理

  1. customAfter leaving
  2. waitto stand for 2 hours at room temperature
  3. stirringThe resulting mixture was stirred for 40 minutes at room temperature
  4. concentrationconcentrated under reduced pressure
  5. filtrationThe precipitate was filtered off
  6. washwashed carefully with cold water
  7. additiontreated with hot chlorform
  8. customGolden crystals were afforded (0.62 g, 85.5%), m.p. 288-290° C.

出典と根拠

ORDレコード
ord-238ae6d3d5b64f388881ec0f478e52b2
出典データセット
uspto-grants-2000_03
特許番号
US06034246

関連ノート

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