Acetonitrile → HCID 19210610、化合物

HRID 980787ノート

反応式

HRID 980787 の反応式
C(#N)C.[C:4]1([S:10]([NH:13][C:14]2[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][CH:15]=2)(=[O:12])=[O:11])[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.C(N(CC)CC)C.[C:28](Cl)(=[O:35])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>CO.O>[C:4]1([S:10]([N:13]([C:28](=[O:35])[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:14]2[CH:15]=[CH:16][C:17]([CH3:20])=[CH:18][CH:19]=2)(=[O:12])=[O:11])[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

参加物

7

反応物 4

HCID 6342AcetonitrileHCID 7412Benzoyl chlorideHCID 8471TriethylamineHCID 238717N-(4-Methylphenyl)benzenesulfonamide

生成物 1

HCID 19210610HCID 19210610、化合物収率 95.8%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

250 ml of an acetonitrile solution containing 60 g (0.24 mole) of N-benzenesulfonyl-p-toluidine synthesized by the same method as in Synthesis Example 1 and 37 ml (0.27 mole) of triethylamine was cooled to below 10° C. and while maintaining this temperature, 35.8 g (0.26 mole) of benzoyl chloride was added dropwise. After the addition, the mixture was further reacted at room temperature for 30 minutes. The reaction mixture was then added to 1 liter of water. The precipitate was collected by filtration, washed with water and then with methanol to give 80.8 g (0.23 mole) of the captioned compound.

後処理

  1. temperaturewas cooled to below 10° C.
  2. additionwas added dropwise
  3. additionAfter the addition
  4. customthe mixture was further reacted at room temperature for 30 minutes
  5. filtrationThe precipitate was collected by filtration
  6. washwashed with water

出典と根拠

ORDレコード
ord-b41d6d023c6640419aab9aa37296d3f7
出典データセット
uspto-grants-1987_01
特許番号
US04639408

反応ノート

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