HCID 86697964, 화합물 → HCID 68360001, 화합물

HRID 518796

반응식

HRID 518796 반응식
[I-].[CH3:2][N+:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-])=O)=[C:11]([O:18][CH:19]([CH3:21])[CH3:20])[CH:10]=2)=[CH:5][CH:4]=1.[H][H]>CO.O.[Pt]=O>[CH3:2][N:3]1[CH2:8][CH2:7][CH:6]([C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[C:11]([O:18][CH:19]([CH3:21])[CH3:20])[CH:10]=2)[CH2:5][CH2:4]1

참가 물질

5

반응물 2

HCID 86697964HCID 86697964, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 68360001HCID 68360001, 화합물수율 96.7%

시약·촉매·용매 2

HCID 86587499Platinum oxide monohydrate촉매HCID 887Methanol용매

실험 절차

A solution of 10 g of 1-methyl-4-[4-nitro-3-(propan-2-yloxy)phenyl]pyridinium iodide in 280 ml of methanol is hydrogenated in an autoclave on 2.9 g of platinum oxide hydrate, at a hydrogen pressure of 15 bar and at ambient temperature for 4 h. The catalyst is removed by filtration on Clarcel and the mixture is concentrated under vacuum. The residue is taken up in 200 ml of ethyl acetate and washed with 200 ml of 1M sodium hydroxide and then with a saturated sodium chloride solution. The organic phase is dried over magnesium sulfate and concentrated under vacuum, so as to obtain 6.0 g of 4-(1-methylpiperidin-4-yl)-2-(propan-2-yloxy)aniline.

후처리

  1. customThe catalyst is removed by filtration on Clarcel
  2. concentrationthe mixture is concentrated under vacuum
  3. washwashed with 200 ml of 1M sodium hydroxide
  4. dry with materialThe organic phase is dried over magnesium sulfate
  5. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-946ca97885874ef1b5b284a4e52a64f0
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115140B2

연결된 노트

불러오는 중…