Hydrochloric Acid → 2-Azido-5-cyano-4-methylamino-pyrimidine

HRID 3161노트

반응식

HRID 3161 반응식
[C:1]([C:3]1[C:4]([NH:11][CH3:12])=[N:5][C:6]([NH:9][NH2:10])=[N:7][CH:8]=1)#[N:2].Cl.[N:14]([O-])=O.[Na+]>O>[N:9]([C:6]1[N:5]=[C:4]([NH:11][CH3:12])[C:3]([C:1]#[N:2])=[CH:8][N:7]=1)=[N+:10]=[N-:14]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 218527585-Cyano-2-hydrazino-4-methylamino-pyrimidineHCID 23668193Sodium Nitrite

생성물 1

HCID 218527592-Azido-5-cyano-4-methylamino-pyrimidine수율 96.8%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
5 °C

실험 절차

To a cold (5° C.) solution of 5-cyano-2-hydrazino-4-methylamino-pyrimidine (21.7 g) from Example 4 in a mixture of water (260 mL) and concentrated HCl (26.5 mL) was added dropwise a solution of NaNO2 (10.03 g) in water (25 mL) with overhead mechanical stirring. A white precipitate formed and after the addition was completed, the reaction was stirred for an additional 20 minutes at 5° C. The insoluble product was filtered and washed with cold water to give 22.4 g of the title compound after drying at 23° C. under high vacuum overnight. Crystallization from ethanol provided an analytically pure sample of 2-azido-5-cyano-4-methylamino-pyrimidine; mp 225°-230° C.

후처리

  1. customA white precipitate formed
  2. additionafter the addition
  3. filtrationThe insoluble product was filtered
  4. washwashed with cold water

출처 및 근거

ORD 기록
ord-3c865d11870445439885fc69ae3775bc
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733914

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