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Diethyl Pyrocarbonate → HCID 57847162, 화합물

HRID 1009938
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HRID 1009938 반응식
[CH3:1][C@:2]12[CH2:14][CH2:13][NH:12][C@H:11]1[C:10]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:4][C@H:3]2[C:15]1[CH:19]=[CH:18][S:17][CH:16]=1.[C:20]([NH:28][C@@H:29]1[CH2:34][CH2:33][CH2:32][CH2:31][C@@H:30]1[C:35](O)=[O:36])(=[O:27])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(N(CC)CC)C.CCOC(OC(OCC)=O)=O.C(=O)([O-])O.[Na+]>O1CCCC1.C(#N)C>[CH3:1][C@@:2]12[CH2:14][CH2:13][N:12]([C:35]([C@H:30]3[CH2:31][CH2:32][CH2:33][CH2:34][C@H:29]3[NH:28][C:20](=[O:27])[C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)=[O:36])[C@@H:11]1[C:10]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:4][C@@H:3]2[C:15]1[CH:19]=[CH:18][S:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 3051Diethyl PyrocarbonateHCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 1268229(+)-cis-2-Benzamidocyclohexanecarboxylic AcidHCID 57846949HCID 57846949, 화합물

생성물 1

HCID 57847162HCID 57847162, 화합물수율 8%

시약·촉매·용매

2
HCID 6342Acetonitrile용매HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of (3aS*,4R*,9bR)-3a-methyl-4-(3-thienyl)-2,3,3a,4,5,9b-hexahydro-1H-pyrrolo[3,2-c]quinoline (750 mg, 2.77 mmol), (1S,2R)-2-(benzoylamino)cyclohexanecarboxylic acid (685 mg, 2.77 mmol), triethylamine (606 mg, 6.10 mmol), acetonitrile (14 ml) and tetrahydrofuran (14 ml) was added DEPC (500 mg, 3.05 mmol) under ice-cooling, and the mixture was stirred for 10 min. The mixture was allowed to return to room temperature and stirred for 12 hrs. Saturated aqueous sodium hydrogen carbonate solution was added to the reaction mixture and the mixture was extracted with ethyl acetate. The extract was dried (over anhydrous Na2SO4), and the solvent was evaporated under reduced pressure. The residue was subjected to column chromatography using silica gel (100 g), and eluted with hexane-ethyl acetate (4:1-1:1, v/v) to give the title compound (3aR,4R,9bR) (110 mg, 8%) as an amorphous form from the first eluted fraction.

후처리

  1. temperaturecooling
  2. customto return to room temperature
  3. stirringstirred for 12 hrs
  4. extractionthe mixture was extracted with ethyl acetate
  5. dry with materialThe extract was dried (over anhydrous Na2SO4)
  6. customthe solvent was evaporated under reduced pressure
  7. washeluted with hexane-ethyl acetate (4:1-1:1

출처 및 근거

ORD 기록
ord-e92734e20b8649ac91afdae978d8ae65
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07973163B2

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