6,6-Dimethyl-2-nitro-6,7-dihydro-4H-pyrazolo[5,1-c][1,4]oxazine → 6,6-Dimethyl-6,7-dihydro-4H-pyrazolo[5,1-c][1,4]oxazin-2-amine

HRID 407748ノート

反応式

HRID 407748 の反応式
[CH3:1][C:2]1([CH3:14])[O:7][CH2:6][C:5]2=[CH:8][C:9]([N+:11]([O-])=O)=[N:10][N:4]2[CH2:3]1>[Pd].CO>[CH3:1][C:2]1([CH3:14])[O:7][CH2:6][C:5]2=[CH:8][C:9]([NH2:11])=[N:10][N:4]2[CH2:3]1

参加物

4

反応物 1

HCID 866840186,6-Dimethyl-2-nitro-6,7-dihydro-4H-pyrazolo[5,1-c][1,4]oxazine

生成物 1

HCID 866840196,6-Dimethyl-6,7-dihydro-4H-pyrazolo[5,1-c][1,4]oxazin-2-amine収率 93%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A 50-mL single-neck round-bottomed flask was purged with nitrogen and charged with 139c (0.21 g, 1.25 mmol), 10% palladium on carbon (50% wet, 125 mg), and methanol (10 mL). The mixture was evacuated, charged with hydrogen gas, and stirred at room temperature for 2 h. The hydrogen was then evacuated and nitrogen was charged into the flask. The catalyst was removed by filtration through a pad of CELITE® and the filtrate was concentrated under reduced pressure to afford 139d (167 mg, 93%). MS-ESI: [M+H]+ 168.1

後処理

  1. customA 50-mL single-neck round-bottomed flask was purged with nitrogen
  2. customThe mixture was evacuated
  3. additioncharged with hydrogen gas
  4. customThe hydrogen was then evacuated
  5. additionnitrogen was charged into the flask
  6. customThe catalyst was removed by filtration through a pad of CELITE®
  7. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-5d4795e9c0d94638ad1760387e07c6e7
出典データセット
uspto-grants-2014_06
特許番号
US08754077B2

反応ノート

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