Sodium Hydroxide → HCID 178515324、化合物

HRID 627472

反応式

HRID 627472 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 min. 50% NaOH and conc. NH4OH solution were added until pH was 9. Some gummy dark brown material formed. After the addition of CH2Cl2, the gummy material became fluffy solid. This solid was filtered, washed with water and Et2O, and air dried to give 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. customSome gummy dark brown material formed
  4. filtrationThis solid was filtered
  5. washwashed with water and Et2O, and air
  6. customdried

出典と根拠

ORDレコード
ord-1929ab8ba3eb4739a08d589c4e9fc9ad
出典データセット
uspto-grants-2016_04
特許番号
US09309222B2

関連ノート

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