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Water → 1-[2-(3,5-Bis-trifluoromethyl-benzenesulfonylamino)-2-oxo-(4-chloro-phenyl)-ethyl]-piperidine-4-carboxylic acid cyclohexylamide

HRID 1455562
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HRID 1455562 반응식
C(N(CC)CC)C.[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([CH:15]([N:19]2[CH2:24][CH2:23][CH:22]([C:25](=[O:33])[NH:26][CH:27]3[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]3)[CH2:21][CH2:20]2)[C:16](O)=[O:17])=[CH:11][CH:10]=1.[F:34][C:35]([F:51])([F:50])[C:36]1[CH:37]=[C:38]([S:46]([NH2:49])(=[O:48])=[O:47])[CH:39]=[C:40]([C:42]([F:45])([F:44])[F:43])[CH:41]=1.O>CN(C1C=CN=CC=1)C.CN(C=O)C>[CH:27]1([NH:26][C:25]([CH:22]2[CH2:21][CH2:20][N:19]([CH:15]([C:12]3[CH:11]=[CH:10][C:9]([Cl:8])=[CH:14][CH:13]=3)[C:16]([NH:49][S:46]([C:38]3[CH:37]=[C:36]([C:35]([F:51])([F:50])[F:34])[CH:41]=[C:40]([C:42]([F:43])([F:44])[F:45])[CH:39]=3)(=[O:47])=[O:48])=[O:17])[CH2:24][CH2:23]2)=[O:33])[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 27831653,5-Bis(trifluoromethyl)benzenesulfonamideHCID 68443812(4-Chlorophenyl)-(4-cyclohexylcarbamoyl-piperidin1-yl)-acetic acid

생성물 1

HCID 865970991-[2-(3,5-Bis-trifluoromethyl-benzenesulfonylamino)-2-oxo-(4-chloro-phenyl)-ethyl]-piperidine-4-carboxylic acid cyclohexylamide

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6228Dimethylformamide용매

실험 절차

140 mg of triethylamine and 0.32 ml of 50% propylphosphonic acid anhydride (solution in DMF) are added to a solution of 150 mg of (4-chlorophenyl)-(4-cyclohexylcarbamoyl-piperidin1-yl)-acetic acid, 174 mg of 3,5-bis(trifluoromethyl)-benzenesulfonamide and 24 mg of DMAP in 6 ml of anhydrous DMF at 10°. The mixture obtained is stirred for ca. 60 hours at RT, solvent is evaporated off and the evaporation residue obtained is treated with EtAc and H2O. Two phases obtained are separated and the organic layer obtained is washed, dried and solvent is evaporated. The evaporation residue obtained is subjected to chromatography on silica gel. 1-[2-(3,5-Bis-trifluoromethyl-benzenesulfonylamino)-2-oxo-(4-chloro-phenyl)-ethyl]-piperidine-4-carboxylic acid cyclohexylamide is obtained.

후처리

  1. customThe mixture obtained
  2. customsolvent is evaporated off
  3. customthe evaporation residue obtained
  4. customTwo phases obtained
  5. customare separated
  6. customthe organic layer obtained
  7. washis washed
  8. customdried
  9. customsolvent is evaporated
  10. customThe evaporation residue obtained

출처 및 근거

ORD 기록
ord-75518a2f70ce4c258a06105ea919ee63
출처 데이터셋
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07482462B2

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