Methyl iodide → HCID 86701772, 화합물

HRID 2174128노트

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HRID 2174128 반응식
[C:1]([CH:3]([C:8]1[C:16]([O:17][CH3:18])=[CH:15][C:14]([CH3:19])=[C:13]2[C:9]=1[CH:10]=[CH:11][N:12]2[C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[C:4]([O:6][CH3:7])=[O:5])#[N:2].IC.[C:29](=O)([O-])[O-].[K+].[K+]>CC(C)=O>[C:1]([C:3]([C:8]1[C:16]([O:17][CH3:18])=[CH:15][C:14]([CH3:19])=[C:13]2[C:9]=1[CH:10]=[CH:11][N:12]2[C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])([CH3:29])[C:4]([O:6][CH3:7])=[O:5])#[N:2]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 86701771HCID 86701771, 화합물

생성물 1

HCID 86701772HCID 86701772, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

(±)-tert-Butyl 4-(1-cyano-2-methoxy-2-oxoethyl)-5-methoxy-7-methyl-1H-indole-1-carboxylate (Example 155-C) (1.1 g, 3.07 mmol) was dissolved in acetone (6.14 ml) and then added iodomethane (0.576 ml, 9.21 mmol) followed by potassium carbonate (0.636 g, 4.60 mmol) and stirred at room temperature for 2.5 hours. The reaction was then cooled in an ice bath and quenched with a saturated aqueous solution of ammonium chloride and diluted with DCM. The layers were separated and the organic layer was dried and concentrated to obtain the title compound. MS (ESI+) m/z 373.4 (M+H).

후처리

  1. temperatureThe reaction was then cooled in an ice bath
  2. customquenched with a saturated aqueous solution of ammonium chloride
  3. additiondiluted with DCM
  4. customThe layers were separated
  5. customthe organic layer was dried
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0f6a7c07b9b24f5ab142092c406ade42
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09056874B2

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