Dimethyl Sulfoxide → HCID 58149524, 화합물

HRID 714146노트

반응식

HRID 714146 반응식
CS(C)=O.[I-].[CH3:6][S+](C)(C)=O.[H-].[Na+].[CH3:13][C:14]([CH3:24])([CH3:23])[C:15]([C:17]1[CH:18]=[N:19][CH:20]=[N:21][CH:22]=1)=[O:16]>O1CCCC1>[C:14]([C:15]1([C:17]2[CH:22]=[N:21][CH:20]=[N:19][CH:18]=2)[CH2:6][O:16]1)([CH3:24])([CH3:23])[CH3:13]

참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 24758Sodium hydrideHCID 74498Sulfoxonium, trimethyl-, iodide (1:1)HCID 136456502,2-Dimethyl-1-(pyrimidin-5-yl)propan-1-one

생성물 1

HCID 58149524HCID 58149524, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Under an atmosphere of argon, 10 ml of dimethyl sulphoxide are slowly added dropwise to 0.96 g (4.3 mmol) of trimethylsulphoxonium iodide and 0.17 g of sodium hydride (60%, 4.3 mmol). The reaction mixture is then stirred at room temperature for 15 min, and 0.65 g (3.9 mmol) of 2,2-dimethyl-1-(5-pyrimidinyl)-1-propanone, dissolved in 2 ml of tetrahydrofuran, is added. The reaction mixture is stirred at 50° C. for 90 min. The reaction mixture is then concentrated under reduced pressure, and saturated aqueous sodium chloride solution and ethyl acetate are added to the residue. The organic phase is separated off, dried with sodium sulphate, filtered and concentrated. This gives 0.70 g (99%) of the desired product, which is reacted without further purification.

후처리

  1. additionis added
  2. stirringThe reaction mixture is stirred at 50° C. for 90 min
  3. concentrationThe reaction mixture is then concentrated under reduced pressure, and saturated aqueous sodium chloride solution and ethyl acetate
  4. additionare added to the residue
  5. customThe organic phase is separated off
  6. dry with materialdried with sodium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThis gives 0.70 g (99%) of the desired product, which is reacted without further purification

출처 및 근거

ORD 기록
ord-781c71d9a53842b5a2eb37ac33e4a01f
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187431B2

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