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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
ノート
印刷プレビュー

反応式

HRID 1455562 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-75518a2f70ce4c258a06105ea919ee63
出典データセット
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07482462B2

反応ノート

読み込み中…

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