Sulfamide → 4H-3-Thia-2,4,5-triaza-phenanthrene 3,3-dioxide

HRID 513686

反応式

HRID 513686 の反応式
[NH2:1][C:2]1[C:3]([CH:12]=O)=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[CH:9][CH:8]=[CH:7]2.[S:14](N)([NH2:17])(=[O:16])=[O:15]>N1C=CC=CC=1>[CH:12]1[C:3]2[CH:4]=[CH:5][C:6]3[C:11](=[N:10][CH:9]=[CH:8][CH:7]=3)[C:2]=2[NH:1][S:14](=[O:16])(=[O:15])[N:17]=1

参加物

4

反応物 2

HCID 82267SulfamideHCID 110520988-Aminoquinoline-7-carboxaldehyde

生成物 1

HCID 681833864H-3-Thia-2,4,5-triaza-phenanthrene 3,3-dioxide収率 82.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

8-Amino-quinoline-7-carbaldehyde 404 (100 mg, 0.58 mmol) and sulfamide (558 mg, 5.81 mmol) in pyridine (2 ml) was heated in a microwave at 140° C. for 2 h. After cooling, the mixture was concentrated in vacuo. The crude residue was dissolved in DCM and neutralised with citric acid. The resulting precipitate was collected by filtration and dried to give the title compound (111 mg, 82%) which was used in the next step without further purification.

後処理

  1. temperatureAfter cooling
  2. concentrationthe mixture was concentrated in vacuo
  3. dissolutionThe crude residue was dissolved in DCM and neutralised with citric acid
  4. filtrationThe resulting precipitate was collected by filtration
  5. customdried

出典と根拠

ORDレコード
ord-c2667734589c408597609779491dae32
出典データセット
uspto-grants-2015_08
特許番号
US09102688B2

関連ノート

読み込み中…