Acetic Acid → HCID 563387, 화합물

HRID 68538노트

반응식

HRID 68538 반응식
C([O:3][C:4]([NH:6][C:7](=[O:19])[C:8]([C:17]#[N:18])=[N:9][NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=O)C.C([O-])(=O)C.[Na+].C(O)(=O)C>O>[C:11]1([N:10]2[C:4](=[O:3])[NH:6][C:7](=[O:19])[C:8]([C:17]#[N:18])=[N:9]2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 517045Sodium AcetateHCID 2822520Ethyl[2-cyano-2-(2-phenylhydrazono)acetamido]formate

생성물 1

HCID 563387HCID 563387, 화합물수율 70%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

Intermediate b (21 g, 0.08 mol) and anhydrous sodium acetate (29 g, 0.35 mol) were added to glacial acetic acid (20v/w, 420 mL). The mixture was warmed up to react under reflux for 2 h. After completion of the reaction, the reaction solution was cooled to 0° C. and poured into water (1200 mL). The mixture was stirred for 30 min and filtered by suction. The filtered cake was washed with water and petroleum ether, and dried to produce an orange red solid (12 g) in a yield of 67.8%.

후처리

  1. temperatureThe mixture was warmed up
  2. customto react
  3. temperatureunder reflux for 2 h
  4. customAfter completion of the reaction
  5. filtrationfiltered by suction
  6. washThe filtered cake was washed with water and petroleum ether
  7. customdried

출처 및 근거

ORD 기록
ord-105a12909b6245179ca0ecfa4091af6a
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822465B2

반응 노트

불러오는 중…