Hexane → Zoxamide

HRID 1740555

反応式

HRID 1740555 の反応式
C(=O)(O)[O-].[Na+].Cl.[NH2:7][C:8]([CH3:15])([CH2:13][CH3:14])[C:9](=[O:12])[CH2:10][Cl:11].CCCCCC.[Cl:22][C:23]1[CH:24]=[C:25]([CH:29]=[C:30]([Cl:33])[C:31]=1[CH3:32])[C:26](Cl)=[O:27]>O.O1CCCC1>[Cl:22][C:23]1[CH:24]=[C:25]([CH:29]=[C:30]([Cl:33])[C:31]=1[CH3:32])[C:26]([NH:7][C:8]([CH2:13][CH3:14])([CH3:15])[C:9](=[O:12])[CH2:10][Cl:11])=[O:27]

参加物

7

反応物 4

HCID 8058Hexane2 回HCID 516892Sodium BicarbonateHCID 11127919Benzoyl chloride, 3,5-dichloro-4-methyl-HCID 183720023-Amino-1-chloro-3-methylpentan-2-one hydrochloride

生成物 1

HCID 122087Zoxamide収率 60.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a well-stirred solution of 1.1 g (13.1 mmol) sodium bicarbonate in 15 mL water was added solid 3-amino-1-chloro-3-methyl-2-pentanone hydrochloride (1 g, 5.4 mmoles) portionwise. To the resulting solution was added 15 mL of hexane followed by dropwise addition of a solution of 3,5-dichloro-4-methylbenzoyl chloride (1.2 g, 5.4 mmol) in 1 mL of tetrahydrofuran. Another 15 mL of hexane was added, and the resulting mixture was stirred at room temperature for 2 hours. The reaction mixture was filtered, and the resulting white solid was dried in a vacuum oven yielding 1.1 g of 3,5-dichloro-N-(3-chloro-1-ethyl-1-methyl-2-oxopropyl)-4-methylbenzamide as a white solid (mp 159-161° C.).

後処理

  1. filtrationThe reaction mixture was filtered
  2. customthe resulting white solid was dried in a vacuum oven

出典と根拠

ORDレコード
ord-cd14cce0f0874e2084d8152bac7e8041
出典データセット
uspto-grants-1999_10
特許番号
US05969200

関連ノート

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