Cyanamide → Cyanamide, [2-(methylthio)-4-pyrimidinyl]-

HRID 544574노트

반응식

HRID 544574 반응식
[N:1]#[C:2][NH2:3].CC(C)([O-])C.[K+].N#CN.[K].Cl[C:15]1[CH:20]=[CH:19][N:18]=[C:17]([S:21][CH3:22])[N:16]=1>CN(C=O)C>[C:2]([NH:3][C:15]1[CH:20]=[CH:19][N:18]=[C:17]([S:21][CH3:22])[N:16]=1)#[N:1]

참가 물질

6

반응물 4

HCID 9864CyanamideHCID 971134-Chloro-2-methylthiopyrimidineHCID 23665647Potassium tert-butoxideHCID 8673943220611-80-7

생성물 1

HCID 20458209Cyanamide, [2-(methylthio)-4-pyrimidinyl]-

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Cyanamide (1.05 g.) was added to potassium t-butoxide (2.8 g.) in DMF (10 ml.) with stirring to produce a fine suspension of potassium cyanamide. To this was added 4-chloro-2-methylthiopyrimidine (4 g.) and the mixture stirred at ambient temperature for 17 hours. The DMF was evaporated in vacuo and the residue suspended in water (20 ml.), the pH adjusted to 11 with dilute aqueous sodium hydroxide and the mixture extracted with EtOAc (2×10 ml.). The aqueous layer was separated, acidified to pH 3 with dilute hydrochloric acid and the precipitate collected, washed with water and dried to give 4-cyanoamino-2-methylthiopyrimidine, m.p. 189-191 (decomp.).

후처리

  1. customto produce
  2. stirringthe mixture stirred at ambient temperature for 17 hours
  3. customThe DMF was evaporated in vacuo
  4. extractionthe mixture extracted with EtOAc (2×10 ml.)
  5. customThe aqueous layer was separated
  6. customthe precipitate collected
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-8dadc2229bbf4f4ba3ff64a9a3c06952
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04451463

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