Hydrochloric Acid → 2-(2,6-Difluorobenzamido)-5-(3-(trifluoromethyl)phenyl)thiazole-4-carboxylic acid

HRID 1255128ノート

反応式

HRID 1255128 の反応式
[F:1][C:2]1[CH:29]=[CH:28][CH:27]=[C:26]([F:30])[C:3]=1[C:4]([NH:6][C:7]1[S:8][C:9]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([C:22]([F:25])([F:24])[F:23])[CH:17]=2)=[C:10]([C:12]([O:14]C)=[O:13])[N:11]=1)=[O:5].[OH-].[Na+].Cl>CO>[F:30][C:26]1[CH:27]=[CH:28][CH:29]=[C:2]([F:1])[C:3]=1[C:4]([NH:6][C:7]1[S:8][C:9]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([C:22]([F:23])([F:24])[F:25])[CH:17]=2)=[C:10]([C:12]([OH:14])=[O:13])[N:11]=1)=[O:5]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 24765114Methyl 2-(2,6-difluorobenzamido)-5-(3-(trifluoromethyl)phenyl)thiazole-4-carboxylate

生成物 1

HCID 590044862-(2,6-Difluorobenzamido)-5-(3-(trifluoromethyl)phenyl)thiazole-4-carboxylic acid収率 95%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Into a solution of Compound 35 (884 mg, 2 mmol) in 20 mL of MeOH was added NaOH (400 mg, 10 mmol). The solution was heated to reflux for 1 hour and cooled down to room temperature. The reaction was neutralized with 2N HCl and extracted with Et2O. The combined extracts were washed with water, dried (Na2SO4), filtered and concentrated. Recrystallization from Et2O gave Compound 66 (810 mg, 95%) as a white solid.

後処理

  1. temperatureThe solution was heated
  2. temperatureto reflux for 1 hour
  3. extractionextracted with Et2O
  4. washThe combined extracts were washed with water
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customRecrystallization from Et2O

出典と根拠

ORDレコード
ord-fa1466a6875843c2b2096ea3a47d692d
出典データセット
uspto-grants-2013_06
特許番号
US08455658B2

反応ノート

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