p-Toluenesulfonic acid → 3,4-Dihydro-2H,6H-[1,3]thiazino[3,2-b]isoquinolin-6-one

HRID 261086ノート

反応式

HRID 261086 の反応式
[SH:1][CH2:2][CH2:3][CH2:4][N:5]1[C:10](=[O:11])[C:9]2=[CH:12][CH:13]=[CH:14][CH:15]=[C:8]2[CH2:7][C:6]1=O.C1(C)C=CC(S(O)(=O)=O)=CC=1>ClC1C=CC=CC=1Cl>[O:11]=[C:10]1[C:9]2[CH:12]=[CH:13][CH:14]=[CH:15][C:8]=2[CH:7]=[C:6]2[S:1][CH2:2][CH2:3][CH2:4][N:5]12

参加物

4

反応物 2

HCID 6101p-Toluenesulfonic acidHCID 12593121HCID 12593121、化合物

生成物 1

HCID 1718613,4-Dihydro-2H,6H-[1,3]thiazino[3,2-b]isoquinolin-6-one

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒

実験手順

A mixture of 112 mg. of N-(3-mercaptopropyl)homophthalimide, 172 mg. of p-toluenesulfonic acid, and 4 ml. of o-dichlorobenzene was heated to 120° C. for 30 minutes. After cooling the reaction mixture, the solvent was distilled off from the reaction mixture under reduced pressure and the residue obtained was extracted with 50 ml. of benzene. The extract was washed with water, dried over anhydrous sodium sulfate, and then the solvent was distilled off under reduced pressure. By recrystallizing the residue thus obtained from isopropyl alcohol, 70 mg. of 6-oxo-3,4-dihydro-2H,6H-1,3-thiazino[3,2-b]isoquinoline was obtained.

後処理

  1. additionA mixture of 112 mg
  2. temperatureAfter cooling the reaction mixture
  3. distillationthe solvent was distilled off from the reaction mixture under reduced pressure
  4. customthe residue obtained
  5. extractionwas extracted with 50 ml
  6. washThe extract was washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. distillationthe solvent was distilled off under reduced pressure
  9. customBy recrystallizing the residue
  10. customthus obtained from isopropyl alcohol, 70 mg

出典と根拠

ORDレコード
ord-dbe1b8399d1641448a137de4e7874155
出典データセット
uspto-grants-1979_08
特許番号
US04163844

反応ノート

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