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Methyl iodide → HCID 14638277、化合物

HRID 374083
ノート
印刷プレビュー

反応式

HRID 374083 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 608089HCID 608089、化合物HCID 10942334Sodium Methoxide

生成物 1

HCID 14638277HCID 14638277、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-26b621b8fe4e4dd3972513f3785f7393
出典データセット
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05166343

反応ノート

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