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

HRID 68675ノート

反応式

HRID 68675 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
25 °C

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-ac59e4f677854e1eae203ec6c547c40b
出典データセット
uspto-grants-2014_09
特許番号
US08822447B2

反応ノート

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