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

반응식

HRID 352007 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 21881414Toluene isopropyl alcohol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-44459ba6d2e4470ea54e583d2f7d30cb
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06743920B2

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