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

HRID 574232
ノート
印刷プレビュー

反応式

HRID 574232 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962Water2 回HCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 584423203-Amino-6-methoxy-5-(trifluoromethyl)pyridine-2-carboxylic acid

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-38db66b0176e40dba6a499540d75f996
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09034879B2

反応ノート

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