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Sodium Bicarbonate → HCID 66603654, 화합물

HRID 884503
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HRID 884503 반응식
O=[C:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[O:9])[CH2:4][CH2:3]1.[NH2:18][C:19]1[CH:28]=[CH:27][C:26]([CH2:29][NH:30][C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])=[CH:25][C:20]=1[C:21]([O:23][CH3:24])=[O:22].[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].C([O-])(O)=O.[Na+]>C(Cl)Cl.CC(O)=O>[CH3:36][C:34]([CH3:37])([O:33][C:31]([NH:30][CH2:29][C:26]1[CH:27]=[CH:28][C:19]([NH:18][CH:2]2[CH2:7][CH2:6][N:5]([C:8]([O:10][CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[O:9])[CH2:4][CH2:3]2)=[C:20]([C:21]([O:23][CH3:24])=[O:22])[CH:25]=1)=[O:32])[CH3:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 516892Sodium BicarbonateHCID 643496Benzyl 4-oxopiperidine-1-carboxylate2회HCID 5049666Sodium triacetoxyborohydride2회HCID 60103040Methyl 2-amino-5-((((tert-butoxy)carbonyl)amino)methyl)benzoate

생성물 1

HCID 66603654HCID 66603654, 화합물수율 90.1%

시약·촉매·용매 2

HCID 176
Acetic Acid
용매
HCID 6344Dichloromethane용매2회

실험 절차

A solution of 1.66 g of benzyl 4-oxopiperidine-1-carboxylate and 1 g of methyl 2-amino-5-({[(1,1-dimethylethoxy)carbonyl]amino}methyl)benzoate obtained in stage 5.1 in 20 ml of DCM is added dropwise at AT to a suspension of 2.04 g of NaBH(OAc)3 in a mixture of 20 ml of DCM and 0.41 ml of AcOH. The mixture is stirred at AT for 15 h 00 and then a further 2.04 g of NaBH(OAc)3 are added. After stirring for 6 h 00, 1.66 g of benzyl 4-oxopiperidine-1-carboxylate are added and the mixture is stirred at AT for 48 h 00. A saturated NaHCO3 solution is added and extraction is carried out with DCM. The organic phase is washed with a saturated NaHCO3 solution and twice with a saturated NH4Cl solution. It is dried over Na2SO4 and filtered, and the filtrate is evaporated under reduced pressure. The residue is chromatographed on silica gel, elution being carried out with an AcOEt/heptane mixture, (5/95, v/v) as far as (40/60, v/v), to give 1.6 g of the expected product.

후처리

  1. additionare added
  2. stirringthe mixture is stirred at AT for 48 h 00
  3. extractionextraction
  4. washThe organic phase is washed with a saturated NaHCO3 solution and twice with a saturated NH4Cl solution
  5. dry with materialIt is dried over Na2SO4
  6. filtrationfiltered
  7. customthe filtrate is evaporated under reduced pressure
  8. customThe residue is chromatographed on silica gel, elution

출처 및 근거

ORD 기록
ord-031fe51e1af548c19334ec4405c1d3de
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08242126B2

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