Sodium Hydroxide → HCID 178515324、化合物

HRID 1478506

反応式

HRID 1478506 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([I:11])=[CH:7][C:3]=1[C:4]([OH:6])=O.[F:12][C:13]([F:24])([F:23])[C:14](=O)[CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.CS(O)(=O)=O.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[OH-].[Na+].[NH4+].[OH-]>C(Cl)Cl>[I:11][C:8]1[CH:7]=[C:3]2[C:2](=[CH:10][CH:9]=1)[N:1]=[C:14]([C:13]([F:23])([F:24])[F:12])[C:15]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[C:4]2[OH:6]

参加物

7

反応物 5

HCID 14798Sodium HydroxideHCID 14923Ammonium HydroxideHCID 72911Benzoic acid, 2-amino-5-iodo-HCID 2229581,1,1-Trifluoro-3-phenyl-2-propanone2 回HCID 86584057Phosphorus Pentoxide-Methanesulfonic Acid

生成物 1

HCID 178515324HCID 178515324、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
100 °C

実験手順

A mixture of 2-amino-5-iodobenzoic acid (5.20 g, 19.8 mmol), 1,1,1-trifluoro-3-phenylpropan-2-one (3.95 g, 21.0 mmol), and Eaton's reagent (12 mL) in a sealed tube was heated at 100° C. for 2 hours. More 1,1,1-trifluoro-3-phenylpropan-2-one (1.60 g, 8.50 mmol) was added and the mixture was heated for another 2 hours. The reaction was then cooled to room temperature, ice water was added, and the mixture was stirred vigorously for about 20 minutes. 50% Aqueous NaOH and concentrated NH4OH solutions were added until pH 9. The resulting dark brown gummy material that formed was diluted with DCM which resulted in a solid precipitate that was collected by filtration. The solids were washed with water and Et2O and air dried to provide the title compound.

後処理

  1. temperaturethe mixture was heated for another 2 hours
  2. temperatureThe reaction was then cooled to room temperature
  3. customThe resulting dark brown gummy material that formed
  4. customresulted in a solid precipitate that
  5. filtrationwas collected by filtration
  6. washThe solids were washed with water and Et2O and air
  7. customdried

出典と根拠

ORDレコード
ord-ee02903722fc45adb3f622fc5b987687
出典データセット
uspto-grants-2016_08
特許番号
US09403816B2

関連ノート

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