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Hydrochloric Acid → 2-[1-[[5-methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl]acetyl]-4-piperidinyl]-4-thiazolecarboxylic acid

HRID 660041
ノート
印刷プレビュー

反応式

HRID 660041 の反応式
C([O:3][C:4]([C:6]1[N:7]=[C:8]([CH:11]2[CH2:16][CH2:15][N:14]([C:17](=[O:29])[CH2:18][N:19]3[C:23]([CH3:24])=[CH:22][C:21]([C:25]([F:28])([F:27])[F:26])=[N:20]3)[CH2:13][CH2:12]2)[S:9][CH:10]=1)=[O:5])C.[OH-].[Na+].Cl>CO>[CH3:24][C:23]1[N:19]([CH2:18][C:17]([N:14]2[CH2:15][CH2:16][CH:11]([C:8]3[S:9][CH:10]=[C:6]([C:4]([OH:5])=[O:3])[N:7]=3)[CH2:12][CH2:13]2)=[O:29])[N:20]=[C:21]([C:25]([F:28])([F:26])[F:27])[CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 66911511ethyl-2-[1-[[5-methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl]acetyl]-4-piperidinyl]-4-thiazolecarboxylate2 回

生成物 1

HCID 666014572-[1-[[5-methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl]acetyl]-4-piperidinyl]-4-thiazolecarboxylic acid収率 90.1%

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

A stirred solution of ethyl-2-[1-[[5-methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl]acetyl]-4-piperidinyl]-4-thiazolecarboxylate (13.0 g, 30.2 mmol) (i.e. the product of Example 2, Step B) in methanol (60 mL) was cooled to 0° C. and treated with an aqueous sodium hydroxide solution (1 N, 36.3 mL, 36.3 mmol). The stirred reaction mixture was allowed to warm to room temperature for 5 h. The reaction mixture was cooled again to 0° C. and treated with aqueous hydrochloric acid (1 N, 36.3 mL, 36.3 mmol). The resulting precipitate was collected under filtration, washed with water and dried in a vacuum oven at 100° C. to give 10.95 g of the title compound as a white solid.

後処理

  1. customThe stirred reaction mixture
  2. temperatureThe reaction mixture was cooled again to 0° C.
  3. filtrationThe resulting precipitate was collected under filtration
  4. washwashed with water
  5. customdried in a vacuum oven at 100° C.

出典と根拠

ORDレコード
ord-4ce00a5aa3544c35b5a4fabe6296d098
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084468B2

反応ノート

読み込み中…

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