1-[(2,3-Dimethyl-5-nitro-6-phenoxypyridin-4-yl)amino]-2-methylpropan-2-ol → 1-[(3-Amino-5,6-dimethyl-2-phenoxypyridin-4-yl)amino]-2-methylpropan-2-ol

HRID 352007ノート

反応式

HRID 352007 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[C:6]([NH:9][CH2:10][C:11]([CH3:14])([OH:13])[CH3:12])[C:5]([N+:15]([O-])=O)=[C:4]([O:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[N:3]=1>[Pt].C1(C)C=CC=CC=1.C(O)(C)C>[NH2:15][C:5]1[C:4]([O:18][C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)=[N:3][C:2]([CH3:1])=[C:7]([CH3:8])[C:6]=1[NH:9][CH2:10][C:11]([CH3:12])([OH:13])[CH3:14]

参加物

4

反応物 1

HCID 129912011-[(2,3-Dimethyl-5-nitro-6-phenoxypyridin-4-yl)amino]-2-methylpropan-2-ol

生成物 1

HCID 129912021-[(3-Amino-5,6-dimethyl-2-phenoxypyridin-4-yl)amino]-2-methylpropan-2-ol

試薬・触媒・溶媒 2

HCID 23939Platinum触媒HCID 21881414Toluene isopropyl alcohol溶媒

実験手順

To a 500 ml Parr hydrogenation flask was added 5% platinum on carbon (1.432 g) and a solution of 1-[(2,3-dimethyl-5-nitro-6-phenoxypyridin-4-yl)amino]-2-methylpropan-2-ol in 90/10 toluene/isopropanol (105 ml). The flask was evacuated until the solvent bubbled, and hydrogen was pressured into the flask at 207 kPa. After three evacuation cycles the flask was pressurized with hydrogen to 345 kPa and mixed on a shaker for about 2 hours. The pressure was released, and thin layer chromatography (TLC) monitoring of the reaction mixture indicated complete reaction. The reaction mixture was filtered, and the solvent was removed under reduced pressure. The resulting product was used in the next step.

後処理

  1. customThe flask was evacuated until the solvent
  2. custombubbled
  3. additionmixed on a shaker for about 2 hours
  4. customreaction
  5. filtrationThe reaction mixture was filtered
  6. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-44459ba6d2e4470ea54e583d2f7d30cb
出典データセット
uspto-grants-2004_06
特許番号
US06743920B2

反応ノート

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