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Water → Methyl 3-amino-6-methoxy-5-(trifluoromethyl)picolinate

HRID 574232
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HRID 574232 반응식
[NH2:1][C:2]1[C:3]([C:14]([OH:16])=[O:15])=[N:4][C:5]([O:12][CH3:13])=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.OS(O)(=O)=O.O.[C:23]([O-])(O)=O.[Na+]>CO>[NH2:1][C:2]1[C:3]([C:14]([O:16][CH3:23])=[O:15])=[N:4][C:5]([O:12][CH3:13])=[C:6]([C:8]([F:9])([F:10])[F:11])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 584423203-Amino-6-methoxy-5-(trifluoromethyl)pyridine-2-carboxylic acid

생성물 1

HCID 71743539Methyl 3-amino-6-methoxy-5-(trifluoromethyl)picolinate

시약·촉매·용매 1

HCID 887Methanol
용매

실험 절차

3-Amino-6-methoxy-5-trifluoromethyl-pyridine-2-carboxylic acid (Int. B) 5.5 g, 23.29 mmol) was dissolved in MeOH (90 ml). H2SO4 (6.21 ml, 116 mmol) was added dropwise and the solution was heated to reflux for 4 hours. The reaction mixture was reduced in vacuo to approx. 15 ml and water (15 ml) was added. The pH was adjusted to pH 9 by careful addition of solid NaHCO3. Water (100 ml) was added and the mixture was extracted with DCM. The combined organic extracts were concentrated in vacuo to afford the title compound.

후처리

  1. temperaturethe solution was heated
  2. temperatureto reflux for 4 hours
  3. additionwas added
  4. extractionthe mixture was extracted with DCM
  5. concentrationThe combined organic extracts were concentrated in vacuo

출처 및 근거

ORD 기록
ord-38db66b0176e40dba6a499540d75f996
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09034879B2

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