4-Toluenesulfonyl chloride → HCID 13772004, 화합물

HRID 980835노트

반응식

HRID 980835 반응식
[N+:1]1([O-])[CH:6]=[CH:5][CH:4]=[C:3]2[CH:7]=[CH:8][C:9]3[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=3[C:11](=[O:12])[C:2]=12.S(Cl)(C1C=CC(C)=CC=1)(=O)=[O:19].C(=O)([O-])[O-].[K+].[K+]>C(Cl)(Cl)Cl.O>[O:12]=[C:11]1[C:2]2[NH:1][C:6](=[O:19])[CH:5]=[CH:4][C:3]=2[CH:7]=[CH:8][C:9]2[CH:16]=[CH:15][CH:14]=[CH:13][C:10]1=2

참가 물질

6

반응물 3

HCID 73974-Toluenesulfonyl chlorideHCID 11430Potassium CarbonateHCID 54117372HCID 54117372, 화합물

생성물 1

HCID 13772004HCID 13772004, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

To a solution of 0.75 gram (0.0034 mole) of the N-oxide thus obtained and 0.77 gram (0.0043 mole) of tosyl chloride in 37.5 milliliters of chloroform was added a solution of 0.58 gram (0.0042.mole) of potassium carbonate in 5.8 milliliters of water and the resulting mixture was stirred vigorously at room temperature for about 60 hours. At the end of this time the reaction mixture was washed with 10 percent aqueous sodium hydroxide whereupon a solid precipitated in the chloroform phase. The solid was recovered by filtration and recrystallized from isopropyl alcohol/methanol to obtain purified 1-oxo-benzo[5,6]cyclohepta[1,2-b]pyrid-2(1H)one product, m.p. 195°-196° C. The elemental analyses were as follows:

후처리

  1. washAt the end of this time the reaction mixture was washed with 10 percent aqueous sodium hydroxide whereupon a solid
  2. customprecipitated in the chloroform phase
  3. filtrationThe solid was recovered by filtration
  4. customrecrystallized from isopropyl alcohol/methanol
  5. customto obtain
  6. custompurified 1-oxo-benzo[5,6]cyclohepta[1,2-b]pyrid-2(1H)one product, m.p. 195°-196° C

출처 및 근거

ORD 기록
ord-c0d115e168cb46fdb208f80ebd1e9bd0
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04639457

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