4-Toluenesulfonyl chloride → HCID 13772004、化合物

HRID 980835ノート

反応式

HRID 980835 の反応式
[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

参加物

6

反応物 3

HCID 73974-Toluenesulfonyl chlorideHCID 11430Potassium CarbonateHCID 54117372HCID 54117372、化合物

生成物 1

HCID 13772004HCID 13772004、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-c0d115e168cb46fdb208f80ebd1e9bd0
出典データセット
uspto-grants-1987_01
特許番号
US04639457

反応ノート

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