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Water → 5-(4-Chloro-phenyl)-6-(2,2,2-trifluoro-ethoxy)-2-trifluoromethyl-nicotinic acid

HRID 598248
ノート
印刷プレビュー

反応式

HRID 598248 の反応式
C([O:3][C:4](=[O:22])[C:5]1[CH:10]=[C:9](Br)[C:8]([O:12][CH2:13][C:14]([F:17])([F:16])[F:15])=[N:7][C:6]=1[C:18]([F:21])([F:20])[F:19])C.[Cl:23][C:24]1[CH:29]=[CH:28][C:27](B(O)O)=[CH:26][CH:25]=1.O.[OH-].[Li+]>C(O)C.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C1(C)C=CC=CC=1>[Cl:23][C:24]1[CH:29]=[CH:28][C:27]([C:9]2[C:8]([O:12][CH2:13][C:14]([F:15])([F:16])[F:17])=[N:7][C:6]([C:18]([F:19])([F:20])[F:21])=[C:5]([CH:10]=2)[C:4]([OH:22])=[O:3])=[CH:26][CH:25]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 962Water3 回HCID 3939Lithium Hydroxide2 回HCID 742994-Chlorophenylboronic acidHCID 866347975-Bromo-6-(2,2,2-trifluoro-ethoxy)-2-trifluoromethyl-nicotinic acid ethyl ester

生成物 1

HCID 866348055-(4-Chloro-phenyl)-6-(2,2,2-trifluoro-ethoxy)-2-trifluoromethyl-nicotinic acid

試薬・触媒・溶媒 3

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 702Ethanol溶媒
HCID 1140Toluene溶媒

反応条件

温度
70 °C

実験手順

5-Bromo-6-(2,2,2-trifluoro-ethoxy)-2-trifluoromethyl-nicotinic acid ethyl ester (2 g, 5.05 mmol) was dissolved in ethanol (30 ml). To this solution was added with stirring [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium (II) CH2Cl2 (41.2 mg, 0.05 mmol), 4-chlorophenylboronic acid (828.8 mg, 5.3 mmol), water (4.8 ml) and lithium hydroxide (246.7 mg, 10.1 mmol). This mixture was heated to 70° C. for 2.5 h and cooled to room temperature. Water (12 mL) and lithium hydroxide (370.0 mg, 15.1 mmol) was added and stirred at 70° C. for 0.5 h. The reaction mixture was cooled to room temperature, treated with water (40 ml) and toluene (40 ml) and extracted. The phases were separated, the organic phase extracted with water (30 ml). The combined water phase was acidified with HCl 2N and extracted with ethylacetate. Organic phases were pooled, dried with Na2SO4 and the volatiles removed in vacuo. The residue was dissolved in ethanol (6 ml) and treated with water (12 ml) to give after crystallization the title compound (1.82 g) as light brown crystals; MS (ISN) 398.0 (M−H)−.

後処理

  1. temperaturecooled to room temperature
  2. temperatureThe reaction mixture was cooled to room temperature
  3. extractionextracted
  4. customThe phases were separated
  5. extractionthe organic phase extracted with water (30 ml)
  6. extractionextracted with ethylacetate
  7. dry with materialdried with Na2SO4
  8. customthe volatiles removed in vacuo
  9. dissolutionThe residue was dissolved in ethanol (6 ml)
  10. additiontreated with water (12 ml)
  11. customto give
  12. customafter crystallization the title compound (1.82 g) as light brown crystals

出典と根拠

ORDレコード
ord-77078c99733a4fe9b2e7c729141e0d24
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07897621B2

反応ノート

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