Methanol → 6-Bromo-N-methyl-4-nitropyridin-3-amine

HRID 1907877ノート

反応式

HRID 1907877 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[C:5]([NH:11][CH3:12])=[CH:4][N+:3]=1[O-].P(Br)(Br)Br.O.CO>ClCCl>[Br:1][C:2]1[N:3]=[CH:4][C:5]([NH:11][CH3:12])=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1

参加物

6

反応物 4

HCID 887MethanolHCID 962WaterHCID 24614Phosphorus tribromideHCID 866591292-Bromo-5-(methylamino)-4-nitropyridine 1-oxide

生成物 1

HCID 866591306-Bromo-N-methyl-4-nitropyridin-3-amine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

2-Bromo-5-(methylamino)-4-nitropyridine 1-oxide (10.0 g, 40.4 mmol) in 200 mL dichloromethane was mixed with phosphorous tribromide (10 mL, 106 mmol) in 50 mL dichloromethane at 10° C. and stirred for 10 minutes at ambient temperature. Water and methanol were added and the mixture was extracted with dichloromethane. The organic layers were washed with Na2CO3 (aq.) dried over MgSO4. The residue was triturated with ethanol, filtered and dried at 50° C. i. vac.

後処理

  1. extractionthe mixture was extracted with dichloromethane
  2. washThe organic layers were washed with Na2CO3 (aq.)
  3. dry with materialdried over MgSO4
  4. customThe residue was triturated with ethanol
  5. filtrationfiltered
  6. customdried at 50° C. i

出典と根拠

ORDレコード
ord-61cf86ea9cbb4b66b0127a2a0d12e471
出典データセット
uspto-grants-2013_12
特許番号
US08598190B2

反応ノート

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