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

HRID 1605243노트

반응식

HRID 1605243 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-94ecfe17e6e54d1bb0dedb5b1ad8e602
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03950339

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