Acetonitrile → HCID 19210610, 화합물

HRID 980787노트

반응식

HRID 980787 반응식
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

참가 물질

7

반응물 4

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

생성물 1

HCID 19210610HCID 19210610, 화합물수율 95.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b41d6d023c6640419aab9aa37296d3f7
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04639408

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