Methanol → HCID 68440920, 화합물

HRID 1455555노트

반응식

HRID 1455555 반응식
CCN(C(C)C)C(C)C.[C:10]([O:14][C:15]([N:17]1[CH2:24][CH:23]2[C:25](=[C:26]([C:28](O)=[O:29])[F:27])[CH:19]([CH2:20][CH2:21][CH2:22]2)[CH2:18]1)=[O:16])([CH3:13])([CH3:12])[CH3:11].[Cl:31][C:32]1[S:33][C:34]([Cl:42])=[C:35]([Cl:41])[C:36]=1[S:37]([NH-:40])(=[O:39])=[O:38].CO>CN(C1C=CN=CC=1)C.CC(N(C)C)=O.O1CCOCC1>[C:10]([O:14][C:15]([N:17]1[CH2:18][CH:19]2[C:25](=[C:26]([F:27])[C:28](=[O:29])[NH:40][S:37]([C:36]3[C:35]([Cl:41])=[C:34]([Cl:42])[S:33][C:32]=3[Cl:31])(=[O:38])=[O:39])[CH:23]([CH2:22][CH2:21][CH2:20]2)[CH2:24]1)=[O:16])([CH3:13])([CH3:11])[CH3:12]

참가 물질

8

반응물 4

HCID 887MethanolHCID 81531DiisopropylethylamineHCID 684431693-(1,1-Dimethylethyl) 9-(carboxyfluoromethylene)-3-azabicyclo[3.3.1]nonane-3-carboxylateHCID 86597098HCID 86597098, 화합물

생성물 1

HCID 68440920HCID 68440920, 화합물

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매HCID 312751,4-Dioxane용매HCID 31374Dimethylacetamide용매

실험 절차

69 μl of DIEA are added to a solution of 60 mg of 9-(carboxy-fluoro-methylene)-3-aza-bicyclo[3.3.1]nonane-3-carboxylic acid tert-butyl ester, 71 mg of 2,4,5-trichloro-thiophene-3-sulfonyl amide, 233 μl of PPA and 24 mg of DMAP in 2 ml of DMA, and the mixture obtained is stirred at 40° overnight. The mixture obtained is diluted with 10 ml of EtAc/c-HEX, and washed with 1M NaHSO4 solution. The organic layer obtained is dried and solvent is evaporated. The evaporation residue obtained is subjected to chromatography on silica gel and on Sephadex LH20 (MeOH) and relevant fractions obtained from chromatography are subjected to lyophilisation from dioxane. 9-[1-Fluoro-2-oxo-2-(2,4,5-trichloro-thiophene-3-sulfonylamino)-ethylidene]-3-aza-bicyclo[3.3.1]nonane-3-carboxylic acid tert.-butyl ester in the form of a powder is obtained.

후처리

  1. customthe mixture obtained
  2. customThe mixture obtained
  3. additionis diluted with 10 ml of EtAc/c-HEX
  4. washwashed with 1M NaHSO4 solution
  5. customThe organic layer obtained
  6. customis dried
  7. customsolvent is evaporated
  8. customThe evaporation residue obtained

출처 및 근거

ORD 기록
ord-18b7bf5dd91b40b7bc510b7cfdf6470c
출처 데이터셋
uspto-grants-2009_01
특허 번호
US07482462B2

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