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

HRID 513686

반응식

HRID 513686 반응식
[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

참가 물질

4

반응물 2

HCID 82267SulfamideHCID 110520988-Aminoquinoline-7-carboxaldehyde

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c2667734589c408597609779491dae32
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09102688B2

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