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Methyl iodide → HCID 14638277, 화합물

HRID 1534347
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HRID 1534347 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, 화합물2회HCID 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 8.0g (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 8.75g 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. temperaturethe solution was heated at its
  3. temperaturereflux temperature for three hours
  4. customThe solvent was removed by evaporation under vacuum
  5. customthe solid was separated by filtration
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-49d7b69e4ef642e79173d4ba59964c1e
출처 데이터셋
uspto-grants-1992_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05089493

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