Methyl iodide → HCID 59605958, 화합물

HRID 1922861노트

반응식

HRID 1922861 반응식
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][NH:8]2)=[C:4]([N:11]2[CH2:16][CH2:15][O:14][CH2:13][C@H:12]2[CH3:17])[N:3]=1.CI.[C:20]([O-])([O-])=O.[K+].[K+]>C1COCC1>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH3:20])=[C:4]([N:11]2[CH2:16][CH2:15][O:14][CH2:13][C@H:12]2[CH3:17])[N:3]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodide2회HCID 11430Potassium CarbonateHCID 178461592HCID 178461592, 화합물

생성물 1

HCID 59605958HCID 59605958, 화합물수율 83%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 2-chloro-6-((R)-3-methylmorpholin-4-yl)-9H-purine (635 mg, 2.50 mmol), methyl iodide (187 μL, 3.00 mmol) and K2CO3 (484 mg, 3.50 mmol) in THF (15 mL) were stirred at r.t. for 18 h before further methyl iodide (187 μL, 3.00 mmol) was added. The resulting mixture was allowed to stir for 65 h then concentrated in vacuo. The resulting residue was partitioned between EtOAc and H2O, the organic phase washed with brine, then dried (Na2SO4) and concentrated in vacuo affording the title compound as an off-white solid (552 mg, 83%). LCMS (method H): RT 2.76 min [M+H]+ 268.3

후처리

  1. additionwas added
  2. concentrationthen concentrated in vacuo
  3. customThe resulting residue was partitioned between EtOAc and H2O
  4. washthe organic phase washed with brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-f56e46484c6e411685b9bc25788ca4bc
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08173650B2

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