Water → HCID 58137367、化合物

HRID 1907824ノート

反応式

HRID 1907824 の反応式
[F:1][C:2]([F:6])([F:5])[CH2:3][OH:4].[H-].[Na+].[CH3:9][O:10][C:11]1[N:12]=[N+:13]([O-:21])[C:14]([CH3:20])=[CH:15][C:16]=1[N+]([O-])=O.O>C(Cl)Cl>[CH3:9][O:10][C:11]1[N:12]=[N+:13]([O-:21])[C:14]([CH3:20])=[CH:15][C:16]=1[O:4][CH2:3][C:2]([F:6])([F:5])[F:1]

参加物

6

反応物 4

HCID 962WaterHCID 64092,2,2-TrifluoroethanolHCID 24758Sodium hydrideHCID 64053053-methoxy-6-methyl-4-nitropyridazine 1-oxide

生成物 1

HCID 58137367HCID 58137367、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
55 °C

実験手順

2,2,2-Trifluoroethanol (3 ml) was initially charged at RT and admixed with sodium hydride (403 mg) in portions while cooling with ice. Thereafter, the reaction mixture was heated to 55° C. for 2 h and then 3-methoxy-6-methyl-4-nitropyridazine 1-oxide solution (500 mg, dissolved in 3 ml of 2,2,2-trifluoroethanol) was added dropwise. After stirring at RT for 1 h, the mixture was heated to 55° C. for 2.5 h. After standing at RT overnight, the mixture was admixed with water and DCM. After removing the DCM phase, the aqueous phase was extracted three times with DCM and the combined DCM phases were dried over sodium sulfate, filtered and concentrated. 571 mg of the title compound were obtained.

後処理

  1. temperaturewhile cooling with ice
  2. temperaturethe mixture was heated to 55° C. for 2.5 h
  3. waitAfter standing at RT overnight
  4. customAfter removing the DCM phase
  5. extractionthe aqueous phase was extracted three times with DCM
  6. dry with materialthe combined DCM phases were dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-f4ffcac51f9143c9a94b3129ee6733c7
出典データセット
uspto-grants-2013_12
特許番号
US08598177B2

反応ノート

読み込み中…