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Potassium Carbonate → HCID 57079992, 화합물

HRID 2299620
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HRID 2299620 반응식
C(=O)([O-])[O-].[K+].[K+].[OH:7][C:8]1[CH:44]=[CH:43][C:11]2[CH2:12][CH2:13][CH2:14][CH:15]([N:17]([C:36]([O:38][C:39]([CH3:42])([CH3:41])[CH3:40])=[O:37])[CH2:18][C@H:19]([O:28][Si:29]([CH2:34][CH3:35])([CH2:32][CH3:33])[CH2:30][CH3:31])[CH2:20][O:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH2:16][C:10]=2[CH:9]=1.Br[CH2:46][F:47].C(=O)([O-])O.[Na+]>C(#N)C.CN(C)C=O>[F:47][CH2:46][O:7][C:8]1[CH:44]=[CH:43][C:11]2[CH2:12][CH2:13][CH2:14][CH:15]([N:17]([C:36]([O:38][C:39]([CH3:41])([CH3:40])[CH3:42])=[O:37])[CH2:18][C@H:19]([O:28][Si:29]([CH2:32][CH3:33])([CH2:30][CH3:31])[CH2:34][CH3:35])[CH2:20][O:21][C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=3)[CH2:16][C:10]=2[CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 61108BromofluoromethaneHCID 516892Sodium BicarbonateHCID 57157362HCID 57157362, 화합물

생성물 1

HCID 57079992HCID 57079992, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매
HCID 6342
Acetonitrile
용매

실험 절차

Under nitrogen, to a suspension of potassium carbonate (76 mg) in a mixture of acetonitrile (5 ml) and N,N-dimethylformamide (2 ml) was added N-(3-hydroxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl)-N-[(2S)-3-phenoxy-2-(triethylsilyloxy)propyl]-tert-butoxycarbonylamine (150 mg) at room temperature. After being stirred at the same temperature for 30 minutes, to this one was an excessive amount of bromofluoromethane, and the mixture was stirred for 12 hours. The resulting solution was poured into saturated aqueous sodium hydrogencarbonate, and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=10:1) to give N-(3-fluoromethoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-6-yl)-N-[(2S)-3-phenoxy-2-(triethylsilyloxy)propyl]-tert-butoxycarbonylamine (130 mg).

후처리

  1. stirringthe mixture was stirred for 12 hours
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customevaporated in vacuo
  6. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=10:1)

출처 및 근거

ORD 기록
ord-4656f41331344820b0720dc735d3cdb8
출처 데이터셋
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06495546B1

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