Methyl iodide → HCID 59277705, 화합물

HRID 1097774노트

반응식

HRID 1097774 반응식
I[CH3:2].[O:3]=[S:4]1(=[O:16])[CH2:9][C:8](=O)[C:7]2[CH:11]=[CH:12][CH:13]=[CH:14][C:6]=2[N:5]1[CH3:15].[C:17]([O-:20])([O-])=O.[K+].[K+]>CN(C=O)C>[CH3:15][N:5]1[C:6]2[CH:7]=[CH:11][CH:12]=[CH:13][C:14]=2[C:17](=[O:20])[C:9]([CH3:8])([CH3:2])[S:4]1(=[O:3])=[O:16]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 27375132,2-Dioxo-1-methyl-2,1-benzothiazin-4(3H)-one

생성물 1

HCID 59277705HCID 59277705, 화합물수율 79.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

Iodomethane (187 ul, 426 mg, 3 mmol) is added dropwise to a suspension of 2,2-Dioxo-1-methyl-2,1-benzothiazin-4(3H)-one ([CAS: 7117-31-9], 220 mg, 1 mmol), K2CO3 (1.38 g, 10 mmol) in 3 mL of dry DMF at room temperature. The resulting mixture is stirred at 60° C. After 2 h, the reaction mixture is filtered, and washed with ethyl acetate (20 mL). The combined solution is concentrated and the residue is purified by flash column (ethyl acetate-heptane v/v 10%) and gives the title compound as white solid (190 mg).

후처리

  1. filtrationthe reaction mixture is filtered
  2. washwashed with ethyl acetate (20 mL)
  3. concentrationThe combined solution is concentrated
  4. customthe residue is purified by flash column (ethyl acetate-heptane v/v 10%)

출처 및 근거

ORD 기록
ord-43d21b9309a547dc84ed1ec1af739cd5
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143278B2

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