Sodium Carbonate → (4-Methyl-6-piperonylamino-2-pyrimidinylthio)acetonitrile

HRID 1605243ノート

反応式

HRID 1605243 の反応式
Cl[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([S:9][CH2:10][C:11]#[N:12])[N:3]=1.[CH2:13]([NH2:23])[C:14]1[CH:22]=[CH:21][C:20]2[O:19][CH2:18][O:17][C:16]=2[CH:15]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[O:19]1[C:20]2[CH:21]=[CH:22][C:14]([CH2:13][NH:23][C:2]3[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([S:9][CH2:10][C:11]#[N:12])[N:3]=3)=[CH:15][C:16]=2[O:17][CH2:18]1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 75799Benzo-1,3-dioxole-5-methylamineHCID 12228966Acetonitrile, [(4-chloro-6-methyl-2-pyrimidinyl)thio]-

生成物 1

HCID 12228971(4-Methyl-6-piperonylamino-2-pyrimidinylthio)acetonitrile

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A stirred mixture of 13.93 g. (0.07 mole) of (4-chloro-6-methyl-2-pyrimidinylthio)acetonitrile, 10.5 g. (0.07 mole) of piperonylamine and 7.42 g. (0.07 mole) of sodium carbonate in 100 ml of ethanol was heated under reflux for five hours. The mixture was filtered and the filtrate was cooled in ice. The precipitate thus formed was collected and recrystallized from absolute ethanol to give 15.7 g. of product, m.p. 115°-118°.

後処理

  1. additionA stirred mixture of 13.93 g
  2. temperatureunder reflux for five hours
  3. filtrationThe mixture was filtered
  4. temperaturethe filtrate was cooled in ice
  5. customThe precipitate thus formed
  6. customwas collected
  7. customrecrystallized from absolute ethanol
  8. customto give 15.7 g

出典と根拠

ORDレコード
ord-94ecfe17e6e54d1bb0dedb5b1ad8e602
出典データセット
uspto-grants-1976_04
特許番号
US03950339

反応ノート

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