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Hydrochloric Acid → (R)-3-(4-isopropyl-benzylcarbamoyl)-4-(4-trifluoromethyl-benzenesulfonyl)-3,4,5,6-tetrahydro-2H-[1,2']bipyrazinyl-5'-carboxylic acid

HRID 908588
ノート
印刷プレビュー

反応式

HRID 908588 の反応式
C[O:2][C:3]([C:5]1[N:6]=[CH:7][C:8]([N:11]2[CH2:16][CH2:15][N:14]([S:17]([C:20]3[CH:25]=[CH:24][C:23]([C:26]([F:29])([F:28])[F:27])=[CH:22][CH:21]=3)(=[O:19])=[O:18])[C@@H:13]([C:30](=[O:42])[NH:31][CH2:32][C:33]3[CH:38]=[CH:37][C:36]([CH:39]([CH3:41])[CH3:40])=[CH:35][CH:34]=3)[CH2:12]2)=[N:9][CH:10]=1)=[O:4].[OH-].[Na+].Cl>O1CCCC1.CO>[CH:39]([C:36]1[CH:35]=[CH:34][C:33]([CH2:32][NH:31][C:30]([C@@H:13]2[N:14]([S:17]([C:20]3[CH:21]=[CH:22][C:23]([C:26]([F:29])([F:28])[F:27])=[CH:24][CH:25]=3)(=[O:19])=[O:18])[CH2:15][CH2:16][N:11]([C:8]3[CH:7]=[N:6][C:5]([C:3]([OH:4])=[O:2])=[CH:10][N:9]=3)[CH2:12]2)=[O:42])=[CH:38][CH:37]=1)([CH3:41])[CH3:40]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 59703851(R)-3-(4-isopropyl-benzylcarbamoyl)-4-(4-trifluoromethyl-benzenesulfonyl)-3,4,5,6-tetrahydro-2H-[1,2']bipyrazinyl-5'-carboxylic acid methyl ester

生成物 1

HCID 25055802(R)-3-(4-isopropyl-benzylcarbamoyl)-4-(4-trifluoromethyl-benzenesulfonyl)-3,4,5,6-tetrahydro-2H-[1,2']bipyrazinyl-5'-carboxylic acid収率 83.3%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixed solution of the compound (75 mg) obtained in Example 8 in tetrahydrofuran (400 μl) and methanol (400 μl) was added, with stirring at room temperature, 2N aqueous sodium hydroxide solution (186 μl). After stirring at room temperature for 30 min, 2N aqueous hydrochloric acid solution (186 μl) was added, and the mixture was concentrated under reduced pressure. Methanol and water were added to the residue, and the mixture was stirred at room temperature. The precipitated crystals were collected by filtration, and dried to give the title compound (61 mg).

後処理

  1. stirringAfter stirring at room temperature for 30 min
  2. concentrationthe mixture was concentrated under reduced pressure
  3. additionMethanol and water were added to the residue
  4. stirringthe mixture was stirred at room temperature
  5. filtrationThe precipitated crystals were collected by filtration
  6. customdried

出典と根拠

ORDレコード
ord-d6743426456f4c32bdecbd9493c750c7
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08017612B2

反応ノート

読み込み中…

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