Dimethyl Sulfate → HCID 59853838, 화합물

HRID 249757노트

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HRID 249757 반응식
[CH2:1]([N:6]1[C:14]2[N:13]=[C:12]([C:15]([F:18])([F:17])[F:16])[NH:11][C:10]=2[C:9](=[S:19])[NH:8][C:7]1=[O:20])[CH2:2][CH2:3][CH2:4][CH3:5].[OH-].[Na+].S(OC)(O[CH3:27])(=O)=O>O>[CH3:27][S:19][C:9]1[C:10]2[NH:11][C:12]([C:15]([F:16])([F:18])[F:17])=[N:13][C:14]=2[N:6]([CH2:1][CH2:2][CH2:3][CH2:4][CH3:5])[C:7](=[O:20])[N:8]=1

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 59853799HCID 59853799, 화합물

생성물 1

HCID 59853838HCID 59853838, 화합물수율 95.6%

시약·촉매·용매 1

HCID 962Water용매

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온도
80 °C

실험 절차

To a mixture of 3-pentyl-6-thioxo-8-(trifluoromethyl)-1,3,6,7-tetrahydro-2H-purin-2-one (0.15 g, 0.49 mmol) in a solution of sodium hydroxide in water (2 M, 2 mL) was added dimethyl sulfate (0.056 mL, 0.59 mmol). The reaction mixture was heated at 80° C. for 1.5 h, quenched with acetic acid and extracted with methylene chloride. The organic layer was dried (MgSO4), concentrate and purified by silica gel chromatography (0-20% EtOAc in hexane) to provide the product as a yellow solid (0.15 g, 95% yield). LCMS calculated for C12H16F3N4OS (M+H): 321.1. found: 321.1.

후처리

  1. customquenched with acetic acid
  2. extractionextracted with methylene chloride
  3. dry with materialThe organic layer was dried (MgSO4)
  4. concentrationconcentrate
  5. custompurified by silica gel chromatography (0-20% EtOAc in hexane)

출처 및 근거

ORD 기록
ord-72e4ad99da134d7591a5194fb4ef1918
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07863285B2

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