(7-nitro-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-3-yl)methanol → (7-amino-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-3-yl)methanol

HRID 970677ノート

反応式

HRID 970677 の反応式
[N+:1]([C:4]1[CH:13]=[N:12][C:11]2[NH:10][CH:9]([CH2:14][OH:15])[CH2:8][O:7][C:6]=2[CH:5]=1)([O-])=O>[Pd].CO>[NH2:1][C:4]1[CH:13]=[N:12][C:11]2[NH:10][CH:9]([CH2:14][OH:15])[CH2:8][O:7][C:6]=2[CH:5]=1

参加物

4

反応物 1

HCID 68703685(7-nitro-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-3-yl)methanol

生成物 1

HCID 59020667(7-amino-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-3-yl)methanol収率 91.5%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

Into a 500 mL round bottom flask were combined (7-nitro-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-3-yl)methanol (0.320 g, 0.00152 mol), 10%-palladium on carbon (0.06 g, 0.0005 mol) and methanol (50 mL). The apparatus was evacuated, then hydrogen was introduced and the mixture was allowed to stir overnight (at 1 atm presuure). The mixture was then filtered through celite and the filtrate was concentrated under vacuum to yield an oil (0.252 g, 89%) which was used directly in the next step without further purification. (0.252 g, 89%) LC-MS 0.29 min. M/Z=181.9 (M+1).

後処理

  1. customInto a 500 mL round bottom flask were combined
  2. customThe apparatus was evacuated
  3. additionhydrogen was introduced
  4. filtrationThe mixture was then filtered through celite
  5. concentrationthe filtrate was concentrated under vacuum

出典と根拠

ORDレコード
ord-fe3ad3924de449f4a5ccb0009841f9ea
出典データセット
uspto-grants-2007_12
特許番号
US07312233B2

反応ノート

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