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Sodium Bicarbonate → HCID 58864429, 화합물

HRID 2355881
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HRID 2355881 반응식
[CH3:1][O:2][C:3](=[O:27])[C@H:4]([NH:16]C(OCC1C=CC=CC=1)=O)[CH2:5][C:6]1[CH:15]=[CH:14][C:9]2[NH:10][C:11](=[O:13])[O:12][C:8]=2[CH:7]=1.C(=O)(O)[O-].[Na+]>C(O)=O.CO.[Pd].C(OCC)(=O)C.C1(C)C=CC=CC=1.C(O)C>[CH3:1][O:2][C:3](=[O:27])[C@H:4]([NH2:16])[CH2:5][C:6]1[CH:15]=[CH:14][C:9]2[NH:10][C:11](=[O:13])[O:12][C:8]=2[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 2

HCID 516892Sodium BicarbonateHCID 25136281HCID 25136281, 화합물

생성물 1

HCID 58864429HCID 58864429, 화합물

시약·촉매·용매 6

HCID 23938Palladium촉매HCID 284Formic Acid용매2회HCID 702Ethanol용매
HCID 887
Methanol
용매
4회
HCID 1140Toluene용매
HCID 8857Ethyl Acetate용매

실험 절차

A solution of (R)-2-benzyloxycarbonylamino-3-(2-oxo-2,3-dihydro-benzooxazol-6-yl)-propionic acid methyl ester (310 mg) in 4.4% formic acid in methanol (20 ml, freshly prepared in degassed methanol) was added via cannula to a suspension of 10% palladium on charcoal in 4.4% formic acid in methanol (20 ml, freshly prepared in degassed methanol). The resulting mixture was stirred at room temperature for 4 h. After filtration through a pad of celite, the solvents were removed in vacuo giving a tan solid. The solid was dissolved in a mixture of ethyl acetate (50 mL), toluene (10 mL) and ethanol (40 ml), and solid sodium bicarbonate (3.1 g) was added. The mixture was stirred at room temperature for 2 h and filtered. Solvents were removed in vacuo to afford the title compound.

후처리

  1. filtrationAfter filtration through a pad of celite
  2. customthe solvents were removed in vacuo
  3. customgiving a tan solid
  4. additionwas added
  5. stirringThe mixture was stirred at room temperature for 2 h
  6. filtrationfiltered
  7. customSolvents were removed in vacuo

출처 및 근거

ORD 기록
ord-13034f6e5acc48bd812124233db4580d
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07754732B2

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