Hydrochloric Acid → HCID 57972811, 화합물

HRID 661459노트

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HRID 661459 반응식
C([O:3][C:4](=[O:10])[CH2:5][C@H:6]([NH2:9])[CH2:7][CH3:8])C.Br[C:12]1[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+].Cl>[Cu](I)I.C(OCC)(=O)C.O.CN(C)C=O>[F:19][C:18]([F:21])([F:20])[C:15]1[CH:16]=[CH:17][C:12]([NH:9][C@H:6]([CH2:7][CH3:8])[CH2:5][C:4]([OH:3])=[O:10])=[CH:13][CH:14]=1

참가 물질

9

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 67872Benzene, 1-bromo-4-(trifluoromethyl)-HCID 11788640HCID 11788640, 화합물

생성물 1

HCID 57972811HCID 57972811, 화합물수율 40.3%

시약·촉매·용매 4

HCID 83717Copper iodide촉매HCID 962Water용매2회HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
100 °C

실험 절차

(R)-3-Aminovaleric acid ethyl ester (0.5 g), 4-bromobenzotrifluoride (0.62 g), copper iodide (0.053 g), potassium carbonate (1.14 g) and water (0.5 ml) were added to dimethylformamide (5 ml) and the mixture was sealed under nitrogen atmosphere and stirred at 100° C. for 3 days. The mixture was cooled, water and ethyl acetate were added to the mixture, and the pH of the mixture was adjusted to about 3 or less with addition of 2N HCl. The organic layer was separated, dried over magnesium sulfate and concentrated at reduced pressure. The resulting residue was purified by column chromatography to give the titled compound (0.29 g, yield 40.3%). MS (APCI) m/z: 262 [M+H]+.

후처리

  1. customthe mixture was sealed under nitrogen atmosphere
  2. temperatureThe mixture was cooled
  3. customThe organic layer was separated
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated at reduced pressure
  6. customThe resulting residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-fa6ec3c00cb0478f81e8cf7948ef838a
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084611B2

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