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

HRID 908582노트

반응식

HRID 908582 반응식
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]

참가 물질

5

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-63206d1913fe41f1bf051644b9587814
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08017612B2

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