Triethylamine → 1-Methyl-4-oxo-1,4-dihydroquinol-3-yl 1-butanesulphonate

HRID 358670노트

반응식

HRID 358670 반응식
[OH:1][C:2]1[C:11](=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]([CH3:13])[CH:3]=1.C(N(CC)CC)C.[CH2:21]([S:25](Cl)(=[O:27])=[O:26])[CH2:22][CH2:23][CH3:24]>ClCCl>[CH2:21]([S:25]([O:1][C:2]1[C:11](=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]([CH3:13])[CH:3]=1)(=[O:27])=[O:26])[CH2:22][CH2:23][CH3:24]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 754301-Butanesulfonyl chlorideHCID 5900784(1H)-Quinolinone, 3-hydroxy-1-methyl-

생성물 1

HCID 231280791-Methyl-4-oxo-1,4-dihydroquinol-3-yl 1-butanesulphonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-Hydroxy-1-methyl-4-quinolone (3 g) was suspended in dichloromethane (200 ml), triethylamine (5.6 ml) was added to the suspension and the mixture was stirred at ambient temperature for hour. 1 -Butanesulphonyl chloride (2.6 ml) was added to the suspension, the mixture stirred for 90 minutes and then left to stand overnight. The resultant mixture was washed with water (400 ml), aqueous sodium hydroxide (1M, 400 ml) and then further water (3×300 ml). The dichloromethane layer was dried over magnesium sulphate and evaporated to give a solid which was crystallised from methanol (100 ml) to give the novel compound 1-methyl-4-oxo-1,4-dihydroquinol-3-yl 1-butanesulphonate, m.p. 143°-144°.

후처리

  1. stirringthe mixture stirred for 90 minutes
  2. waitleft
  3. washThe resultant mixture was washed with water (400 ml), aqueous sodium hydroxide (1M, 400 ml)
  4. dry with materialThe dichloromethane layer was dried over magnesium sulphate
  5. customevaporated
  6. customto give a solid which
  7. customwas crystallised from methanol (100 ml)

출처 및 근거

ORD 기록
ord-fb8da9ab9d124799922b95279e548b65
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04997840

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