Tetrahydrofuran → Ethyl-[5-(2-isopropyl-4,5-dimethoxy-benzyl)-2-methanesulfonyl-pyrimidin-4-yl]-amine

HRID 2266074노트

반응식

HRID 2266074 반응식
[CH2:1]([NH:3][C:4]1[C:9]([CH2:10][C:11]2[CH:16]=[C:15]([O:17][CH3:18])[C:14]([O:19][CH3:20])=[CH:13][C:12]=2[CH:21]([CH3:23])[CH3:22])=[CH:8][N:7]=[C:6](SC)[N:5]=1)[CH3:2].[CH2:26]1COCC1.O[O:32][S:33]([O-:35])=O.[K+]>O>[CH2:1]([NH:3][C:4]1[C:9]([CH2:10][C:11]2[CH:16]=[C:15]([O:17][CH3:18])[C:14]([O:19][CH3:20])=[CH:13][C:12]=2[CH:21]([CH3:22])[CH3:23])=[CH:8][N:7]=[C:6]([S:33]([CH3:26])(=[O:35])=[O:32])[N:5]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 23707502Potassium hydroxy sulfiteHCID 59598719Ethyl-[5-(2-isopropyl-4,5-dimethoxy-benzyl)-2-methylsulfanyl-pyrimidin-4-yl]-amine

생성물 1

HCID 59598536Ethyl-[5-(2-isopropyl-4,5-dimethoxy-benzyl)-2-methanesulfonyl-pyrimidin-4-yl]-amine수율 92%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To a solution of ethyl-[5-(2-isopropyl-4,5-dimethoxy-benzyl)-2-methylsulfanyl-pyrimidin-4-yl]-amine (0.129 g, 0.4 mmol) in 20 mL 1:1 1H2O/THF was added OXONE® (0.461 g, 0.8 mmol) in 4.0 mL H2O. After 2 hours, 50 mL H2O was added and the mixture was extracted with ethyl acetate, washed with H2O and washed with brine. The combined organic layers were dried over Na2SO4, filtered and concentrated in vacuo to give ethyl-[5-(2-isopropyl-4,5-dimethoxy-benzyl)-2-methanesulfonyl-pyrimidin-4-yl]-amine (0.131 g, 92%) as a white foam.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washwashed with H2O
  3. washwashed with brine
  4. dry with materialThe combined organic layers were dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3d3f0c9e15ed4d6a916a114453bdd281
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07858632B2

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