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Potassium Carbonate → cis-(2-Benzyloxyamino-cyclohexyl)-acetic acid ethyl ester

HRID 580878
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HRID 580878 반응식
[CH2:1]([O:3][C:4](=[O:21])[CH2:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][C:7]1=[N:12][O:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH3:2].[BH3-]C#N.[Na+].C([O-])(O)=O.[Na+].C([O-])([O-])=O.[K+].[K+]>C(O)(=O)C>[CH2:1]([O:3][C:4](=[O:21])[CH2:5][C@@H:6]1[CH2:11][CH2:10][CH2:9][CH2:8][C@@H:7]1[NH:12][O:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH3:2].[CH2:1]([O:3][C:4](=[O:21])[CH2:5][C@@H:6]1[CH2:11][CH2:10][CH2:9][CH2:8][C@H:7]1[NH:12][O:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 516892Sodium BicarbonateHCID 5003444Sodium cyanoborohydrideHCID 54396605(2-Benzyloxyimino-cyclohexyl)-acetic acid ethyl ester

생성물 2

HCID 54235283cis-(2-Benzyloxyamino-cyclohexyl)-acetic acid ethyl ester수율 43%
HCID 54235284
trans-(2-Benzyloxyamino-cyclohexyl)-acetic acid ethyl ester
수율 11%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

(2-Benzyloxyimino-cyclohexyl)-acetic acid ethyl ester (4.66 g, 16.1 mmol) was taken up in 15 mL of acetic acid (AcOH) and NaBH3CN and stirred for 72 hours. Reaction was poured into NaHCO3 and extracted into EtOAc (3×30 mL). The combined organic layers were washed once with brine, dried over Na2SO4, filtered, and concentrated. The clear oil was dissolved in 50 mL of MeOH and K2CO3 (5.55 g, 40.2 mmol) was added and the reaction stirred for 12 hours. The reaction was concentrated, the residue taken up in CHCl3, filtered, and concentrated. Purification by chromatography (SiO2, 4:1 hexanes/EtOAc) afforded 1.72 g (43%) of cis-(2-benzyloxyamino-cyclohexyl)-acetic acid ethyl ester and 0.441 g (11%) of trans-(2-benzyloxyamino-cyclohexyl)-acetic acid ethyl ester.

후처리

  1. customReaction
  2. extractionextracted into EtOAc (3×30 mL)
  3. washThe combined organic layers were washed once with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. dissolutionThe clear oil was dissolved in 50 mL of MeOH
  8. concentrationThe reaction was concentrated
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customPurification by chromatography (SiO2, 4:1 hexanes/EtOAc)

출처 및 근거

ORD 기록
ord-86065eba84324f649754c1e222f78a51
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05919790

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