HCID 178470035, 화합물 → HCID 178516647, 화합물

HRID 639624

반응식

HRID 639624 반응식
C(OC(=O)[C:5]1[C:10]([OH:11])=[CH:9][C:8]([C:12]([F:15])([F:14])[F:13])=[N:7][C:6]=1[OH:16])C>Cl>[F:15][C:12]([F:13])([F:14])[C:8]1[N:7]=[C:6]([OH:16])[CH:5]=[C:10]([OH:11])[CH:9]=1

참가 물질

3

반응물 1

HCID 178470035HCID 178470035, 화합물

생성물 1

HCID 178516647HCID 178516647, 화합물수율 99.5%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
100 °C

실험 절차

2,4-Dihydroxy-6-trifluoromethyl-nicotinic acid ethyl ester (62 g/247 mmols) was added in several portions over 30 mins to 6M HCl(aq) (620 mls) at reflux. The resulting mixture was then heated at 100° C. overnight with vigorous stirring to obtain complete solution. The solution was then allowed to cool and concentrated in vacuo to a white solid. This was slurried in water (250 mls) and adjusted to pH 7 with conc. ammonia to get heavy white suspension. The resulting solid was collected by filtration, rinsed through with fresh water, and dried to provide the title compound (44.0 g) as a white solid.

후처리

  1. temperatureat reflux
  2. customto obtain complete solution
  3. temperatureto cool
  4. concentrationconcentrated in vacuo to a white solid
  5. customto get heavy white suspension
  6. filtrationThe resulting solid was collected by filtration
  7. washrinsed through with fresh water
  8. customdried

출처 및 근거

ORD 기록
ord-f3aba04b1d624006845308eb4c12e6ca
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07691877B2

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