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Methyl iodide → HCID 14638277, 화합물

HRID 374083
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HRID 374083 반응식
[Cl:1][C:2]1[C:7]2[O:8][CH2:9][C:10](=[O:12])[NH:11][C:6]=2[N:5]=[C:4]([CH3:13])[N:3]=1.[CH3:14]I.C[O-].[Na+]>CO>[Cl:1][C:2]1[C:7]2[O:8][CH2:9][C:10](=[O:12])[N:11]([CH3:14])[C:6]=2[N:5]=[C:4]([CH3:13])[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 608089HCID 608089, 화합물HCID 10942334Sodium Methoxide

생성물 1

HCID 14638277HCID 14638277, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Using the method of Sazonov, et al., Khimiya Geterotsiklicheskikh Soedinenii, 9, 1285-1288 (1972), 4-chloro-6,7-dihydro-2-methyl-8H-pyrimido[5,4-b ][1,4]oxazin-7-one was prepared. To a mixture of 8.0 g (0.0402 mole) of 4-chloro-6,7-dihydro-2-methyl-8H-pyrimido [5,4-b]1,4]oxazin-7-one and 17.9 ml of methyl iodide was added 8.75 g of 25% sodium methoxide in 250 ml of methanol, and the solution was heated at its reflux temperature for three hours. The solvent was removed by evaporation under vacuum, and the solid was separated by filtration, washed with water, and dried. The yellow solid was 4-chloro-6,7-dihydro-2,8-dimethylpyrimido[5,4-b][1,4]oxazin-7-one, m.p. 142°-143° C.

후처리

  1. customwas prepared
  2. additionTo a mixture of 8.0 g (0.0402 mole) of 4-chloro-6,7-dihydro-2-methyl-8H-pyrimido
  3. temperaturethe solution was heated at its
  4. temperaturereflux temperature for three hours
  5. customThe solvent was removed by evaporation under vacuum
  6. customthe solid was separated by filtration
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-26b621b8fe4e4dd3972513f3785f7393
출처 데이터셋
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05166343

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