Diisopropyl Ether → (R)-1-(4-trifluoromethyl-benzenesulfonyl)-piperazine-2-carboxylic acid 4-isopropyl-benzylamide hydrochloride

HRID 908582ノート

反応式

HRID 908582 の反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([S:14]([C:17]2[CH:22]=[CH:21][C:20]([C:23]([F:26])([F:25])[F:24])=[CH:19][CH:18]=2)(=[O:16])=[O:15])[C@@H:10]([C:27](=[O:39])[NH:28][CH2:29][C:30]2[CH:35]=[CH:34][C:33]([CH:36]([CH3:38])[CH3:37])=[CH:32][CH:31]=2)[CH2:9]1)=O)(C)(C)C.[ClH:40].C(OCC)(=O)C.C(OC(C)C)(C)C>C(OCC)(=O)C>[ClH:40].[CH:36]([C:33]1[CH:32]=[CH:31][C:30]([CH2:29][NH:28][C:27]([C@H:10]2[CH2:9][NH:8][CH2:13][CH2:12][N:11]2[S:14]([C:17]2[CH:22]=[CH:21][C:20]([C:23]([F:26])([F:24])[F:25])=[CH:19][CH:18]=2)(=[O:16])=[O:15])=[O:39])=[CH:35][CH:34]=1)([CH3:38])[CH3:37]

参加物

5

反応物 3

HCID 7914Diisopropyl EtherHCID 21866389Hydrogen chloride-ethyl acetateHCID 59703719(R)-3-(4-isopropyl-benzylcarbamoyl)-4-(4-trifluoromethyl-benzenesulfonyl)-piperazine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 67410019(R)-1-(4-trifluoromethyl-benzenesulfonyl)-piperazine-2-carboxylic acid 4-isopropyl-benzylamide hydrochloride

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

To a solution of the compound (973 mg) obtained in Step 2 in ethyl acetate (10 ml) was added, with stirring at room temperature, 4N hydrogen chloride/ethyl acetate solution (4.73 ml). After stirring at room temperature for 4 hr, the reaction mixture was concentrated under reduced pressure. Toluene was added to the residue, and the mixture was concentrated again under reduced pressure. The obtained crude crystals were suspended in a mixed solvent of ethyl acetate and diisopropyl ether, collected by filtration and dried to give the title compound (742 mg).

後処理

  1. stirringAfter stirring at room temperature for 4 hr
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. additionToluene was added to the residue
  4. concentrationthe mixture was concentrated again under reduced pressure
  5. customThe obtained crude crystals
  6. filtrationcollected by filtration
  7. customdried

出典と根拠

ORDレコード
ord-63206d1913fe41f1bf051644b9587814
出典データセット
uspto-grants-2011_09
特許番号
US08017612B2

反応ノート

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