Hydrochloric Acid → HCID 72756950、化合物

HRID 132544

反応式

HRID 132544 の反応式
[CH2:1]([O:3][NH2:4])[CH3:2].[C:5]([C:8]1[CH:13]=[CH:12][C:11]([S:14]([NH:17][CH2:18][C:19]2[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=2)(=[O:16])=[O:15])=[CH:10][CH:9]=1)(=O)[CH3:6].Cl.C([O-])(O)=O.[Na+]>CO.O>[CH2:1]([O:3][N:4]=[C:5]([C:8]1[CH:9]=[CH:10][C:11]([S:14]([NH:17][CH2:18][C:19]2[CH:20]=[CH:21][N:22]=[CH:23][CH:24]=2)(=[O:15])=[O:16])=[CH:12][CH:13]=1)[CH3:6])[CH3:2]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 69357Hydroxylamine, O-ethyl-HCID 516892Sodium BicarbonateHCID 64934684-acetyl-N-(pyridin-4-ylmethyl)benzenesulfonamide

生成物 1

HCID 72756950HCID 72756950、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
22.5 °C

実験手順

0.42 g of a 40% strength aqueous O-ethylhydroxylamine solution was added to a solution of 0.4 g (1.3 mmol) of the compound from Example 1 in 20 ml of methanol. Using 10% strength hydrochloric acid, the mixture was acidified to pH 4, and the solution was then stirred at 20-25° C. for about 18 hours. The reaction solution was poured into water and adjusted to pH 8 using NaHCO3. The mixture was then extracted with methyl tert-butyl ether (MtBE), and the combined organic phases were washed with water and dried. Removal of the solvent gave 0.4 g of the title compound as a viscous oil.

後処理

  1. extractionThe mixture was then extracted with methyl tert-butyl ether (MtBE)
  2. washthe combined organic phases were washed with water
  3. customdried
  4. customRemoval of the solvent

出典と根拠

ORDレコード
ord-21f70d2ac52d45769953da9741049837
出典データセット
uspto-grants-2008_06
特許番号
US07388018B2

関連ノート

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