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Benzyl chloroformate → HCID 86590129, 화합물

HRID 1840516
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HRID 1840516 반응식
[CH3:1][C:2]([CH3:22])([O:4][C:5]([NH:7][C@@H:8]([CH2:13][C:14]#[C:15][C:16]1[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=1)[C:9]([O:11][CH3:12])=[O:10])=[O:6])[CH3:3].[H][H].C(=O)([O-])O.[Na+].Cl[C:31]([O:33][CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)=[O:32]>C(O)C.C(O)(=O)C.O1CCCC1.O.C(OCC)(=O)C.[Pd].[Pt]=O>[CH3:3][C:2]([CH3:22])([O:4][C:5]([NH:7][C@@H:8]([CH2:13][CH2:14][CH2:15][CH:16]1[CH2:21][CH2:20][N:19]([C:31]([O:33][CH2:34][C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)=[O:32])[CH2:18][CH2:17]1)[C:9]([O:11][CH3:12])=[O:10])=[O:6])[CH3:1]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

12

반응물 4

HCID 10387Benzyl chloroformateHCID 516892Sodium BicarbonateHCID 86590130HCID 86590130, 화합물HCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 86590129HCID 86590129, 화합물수율 79.1%

시약·촉매·용매 7

HCID 23938Palladium
촉매
HCID 82844Platinum oxide (PtO)촉매
HCID 176Acetic Acid용매
HCID 702Ethanol용매
HCID 962Water용매2회
HCID 8028Tetrahydrofuran용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
0 °C

실험 절차

A mixture of 2.8 g (10.0 mmol) of methyl (S)-2-[[(1,1-dimethylethoxy)carbonyl]amino]-5-pyrid-4-ylpent-4-ynoate and 0.28 g of active 10% palladium-on-charcoal in 20 ml of ethanol is stirred for 3 hours at room temperature under 60 psi of hydrogen. The reaction mixture is filtered and concentrated under reduced pressure. The residue obtained is taken up in 20 ml of acetic acid and stirred for 14 hours in the presence of 0.05 g of platinum oxide, under 60 psi of hydrogen. The reaction mixture is filtered and then concentrated under reduced pressure. The residue obtained is taken up in 10 ml of tetrahydrofuran (THF) and 5 ml of water. This solution is cooled to 0° C., followed by addition of a solution of 3.4 g (40.0 mmol) of sodium hydrogen carbonate in 40 ml of water, and 1.63 ml (12.0 mmol) of benzyl chloroformate are added dropwise. The mixture is allowed to warm to room temperature and the reaction is continued for 4 hours. The reaction mixture is taken up in 200 ml of ethyl acetate and is washed twice with 100 ml of 1N hydrochloric acid solution and then with 100 ml of saturated sodium hydrogen carbonate solution and with 100 ml of saturated sodium chloride solution. The resulting solution is dried over sodium sulphate. The resulting product is filtered and concentrated. The residue obtained is purified by chromatography on a column of silica gel, eluting under pressure with a cyclohexane/ethyl acetate gradient of from 95/5 to 80/20. 3.55 g of methyl (S)-α-[[(1,1-dimethylethoxy)carbonyl]amino]-1-[(phenylmethoxy)carbonyl]piperidine-4-pentanoate are obtained in the form of a viscous oil.

후처리

  1. filtrationThe reaction mixture is filtered
  2. concentrationconcentrated under reduced pressure
  3. customThe residue obtained
  4. filtrationThe reaction mixture is filtered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue obtained
  7. additionare added dropwise
  8. temperatureto warm to room temperature
  9. washis washed twice with 100 ml of 1N hydrochloric acid solution
  10. dry with materialThe resulting solution is dried over sodium sulphate
  11. filtrationThe resulting product is filtered
  12. concentrationconcentrated
  13. customThe residue obtained
  14. customis purified by chromatography on a column of silica gel
  15. washeluting under pressure with a cyclohexane/ethyl acetate gradient of from 95/5 to 80/20

출처 및 근거

ORD 기록
ord-b3f8187a308d4346b93100bed5c9e9c9
출처 데이터셋
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06680329B2

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