O-Xylene → 6-Nitro-1-phenyl-1,2-dihydroindazole-3-thione

HRID 68675노트

반응식

HRID 68675 반응식
[N+:1]([C:4]1[CH:12]=[C:11]2[C:7]([C:8](=O)[NH:9][N:10]2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2].C1(C)C(C)=CC=CC=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:29]>C(OCC)(=O)C>[N+:1]([C:4]1[CH:12]=[C:11]2[C:7]([C:8](=[S:29])[NH:9][N:10]2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2]

참가 물질

5

반응물 3

HCID 7237O-XyleneHCID 14817Phosphorus sulfide (P2S5)HCID 569578826-Nitro-1-phenyl-1,2-dihydroindazol-3-one

생성물 1

HCID 498399766-Nitro-1-phenyl-1,2-dihydroindazole-3-thione

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
25 °C

실험 절차

Into a 250-mL 3-necked round-bottom flask, was placed 6-nitro-1-phenyl-1,2-dihydroindazol-3-one (15 g, 58.82 mmol, 1.00 equiv), xylene (150 mL), P2S5 (52.2 g, 235.14 mmol). The resulting solution was heated to reflux for 40 min in an oil bath. The resulting mixture was then cooled to 25° C. The resulting solution was diluted with ethyl acetate (50 mL). The solids were filtered out to yield 6-nitro-1-phenyl-1,2-dihydroindazole-3-thione as a yellow solid. MS: 272 (MH+).

후처리

  1. customInto a 250-mL 3-necked round-bottom flask, was placed
  2. temperatureThe resulting solution was heated
  3. temperatureto reflux for 40 min in an oil bath
  4. filtrationThe solids were filtered out

출처 및 근거

ORD 기록
ord-ac59e4f677854e1eae203ec6c547c40b
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822447B2

반응 노트

불러오는 중…