Ammonia → 4-Methyl-5-nitrosaccharin

HRID 1599972노트

반응식

HRID 1599972 반응식
[NH3:1].O.C[O:4][C:5]([C:7]1[C:12]([CH3:13])=[C:11]([N+:14]([O-:16])=[O:15])[CH:10]=[CH:9][C:8]=1[S:17](Cl)(=[O:19])=[O:18])=O>O1CCCC1>[CH3:13][C:12]1[C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=[C:8]2[C:7]=1[C:5](=[O:4])[NH:1][S:17]2(=[O:19])=[O:18]

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 962WaterHCID 153345332-Methoxycarbonyl-3-methyl-4-nitrobenzenesulfonyl chloride

생성물 1

HCID 153345344-Methyl-5-nitrosaccharin

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
25 °C

실험 절차

104 ml of 25 percent ammonia solution are initially taken, 100 ml of water are added and a solution of 48.7 g (0.166 mol) of 2-methoxycarbonyl-3-methyl-4-nitrobenzenesulfonyl chloride in 70 ml of tetrahydrofuran is then added dropwise at 10° C. After stirring at 25° C. for three hours, water and THF are largely removed and the residue which remains is stirred with ethyl acetate, filtered off with suction and washed with ethyl acetate. After drying under reduced pressure, 34 g (0.131 mol)=79% of theory of a white solid of m.p.: 312° C. (dec.) are obtained.

후처리

  1. customwater and THF are largely removed
  2. stirringthe residue which remains is stirred with ethyl acetate
  3. filtrationfiltered off with suction
  4. washwashed with ethyl acetate
  5. customAfter drying under reduced pressure, 34 g (0.131 mol)=79% of theory of a white solid of m.p.: 312° C. (dec.)
  6. customare obtained

출처 및 근거

ORD 기록
ord-ec3e47225e444bbdb1271612591fff07
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05744425

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