Sodium Hydroxide → HCID 178492289、化合物

HRID 638235ノート

反応式

HRID 638235 の反応式
[OH-].[Na+].[F:3][C:4]1([F:19])[O:17][C:8]2=[CH:9][C:10]3[N:14]=[C:13]([SH:15])[NH:12][C:11]=3[CH:16]=[C:7]2[O:6][CH:5]1[F:18].Cl.Cl[CH2:22][C:23]1[C:28]([CH3:29])=[C:27]([O:30][CH3:31])[C:26]([CH3:32])=[CH:25][N:24]=1>C(O)C>[F:19][C:4]1([F:3])[O:17][C:8]2=[CH:9][C:10]3[N:14]=[C:13]([S:15][CH2:22][C:23]4[C:28]([CH3:29])=[C:27]([O:30][CH3:31])[C:26]([CH3:32])=[CH:25][N:24]=4)[NH:12][C:11]=3[CH:16]=[C:7]2[O:6][CH:5]1[F:18]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 116942582-(Chloromethyl)-3,5-dimethyl-4-methoxypyridine hydrochlorideHCID 178506022HCID 178506022、化合物

生成物 1

HCID 178492289HCID 178492289、化合物収率 77%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
40 °C

実験手順

6.1 ml of 2M sodium hydroxide solution are added dropwise to a mixture of 1.6 g of 6,6,7-trifluoro-6,7-dihydro-1H-[1,4]-dioxino[2,3-f]benzimidazole-2-thiol and 1.4 g of 2-chloromethyl-4-methoxy-3,5-dimethylpyridine hydrochloride in 40 ml of ethanol at room temperature and the mixture is stirred at 40° C. for 5 h. The solvent is distilled off in vacuo, water is added, the mixture is extracted with methylene chloride, the organic solution is concentrated and the residue is recrystallized from ethanol and water. 1.9 g (77%) of the title compound of m.p. 138°-140° C. are obtained.

後処理

  1. distillationThe solvent is distilled off in vacuo, water
  2. additionis added
  3. extractionthe mixture is extracted with methylene chloride
  4. concentrationthe organic solution is concentrated
  5. customthe residue is recrystallized from ethanol and water

出典と根拠

ORDレコード
ord-70c9a3d34e99416db7d353ede2cbba47
出典データセット
uspto-grants-1985_12
特許番号
US04560693

反応ノート

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