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Carbon Disulfide → HCID 13730272, 화합물

HRID 65205
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HRID 65205 반응식
C([S:4][CH:5]([CH2:21][NH:22][C:23]([O:25][CH2:26][C:27]1[CH:32]=[CH:31][C:30]([N+:33]([O-:35])=[O:34])=[CH:29][CH:28]=1)=[O:24])[CH2:6][NH:7][C:8]([O:10][CH2:11][C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=1)=[O:9])(=O)C.C[O-].[Na+].[C:39](=[S:41])=[S:40].C(O[CH:46]1[NH:49][C:48](=[O:50])[CH:47]1[C@H:51]([O:53][Si:54]([C:57]([CH3:60])([CH3:59])[CH3:58])([CH3:56])[CH3:55])[CH3:52])(=O)C>CO.O1CCCC1.O.C(O)(=O)C>[Si:54]([O:53][C@@H:51]([C@@H:47]1[C@@H:46]([S:40][C:39]([S:4][CH:5]([CH2:6][NH:7][C:8]([O:10][CH2:11][C:12]2[CH:13]=[CH:14][C:15]([N+:18]([O-:20])=[O:19])=[CH:16][CH:17]=2)=[O:9])[CH2:21][NH:22][C:23]([O:25][CH2:26][C:27]2[CH:28]=[CH:29][C:30]([N+:33]([O-:35])=[O:34])=[CH:31][CH:32]=2)=[O:24])=[S:41])[NH:49][C:48]1=[O:50])[CH3:52])([C:57]([CH3:60])([CH3:58])[CH3:59])([CH3:56])[CH3:55]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 6348Carbon DisulfideHCID 10942334Sodium Methoxide2회HCID 130738914-acetoxy-3-[1-(R)-t-butyldimethylsilyloxyethyl)-2-azetidinoneHCID 137302702-Acetylthio-1,3-bis(p-nitrobenzyloxycarbonylamino)propane

생성물 1

HCID 13730272HCID 13730272, 화합물

시약·촉매·용매 4

HCID 176
Acetic Acid
용매
HCID 887Methanol용매2회
HCID 962Water용매
HCID 8028Tetrahydrofuran용매

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온도
-20 °C

실험 절차

5.3 g of 2-acetylthio-1,3-bis(p-nitrobenzyloxycarbonylamino)propane in a mixture of 161 ml of methanol and 40 ml of tetrahydrofuran were cooled to -20° C. To the solution were added 9.95 ml of a methanolic solution of sodium methoxide containing 1 mM of sodium methoxide per 1 ml of methanol. The mixture was stirred at -10° to -15° C. for 30 minutes, after which it was mixed with 0.961 ml of carbon disulphide and stirred at -20° C. for 15 minutes. Then 20 ml of a methanolic solution containing 3.59 g of 4-acetoxy-3-[1-(R)-t-butyldimethylsilyloxyethyl)-2-azetidinone was added to the above mixture and stirred at -20° C. for 1 hour. The mixture was cooled to -50° C. and then poured into a mixture of 20 ml of acetic acid and 200 ml of water. The mixture was extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulphate. The solvent was distilled off and the residue was subjected to medium pressure column chromatography througn silica gel, eluted with 3:1-2:1 by volume mixtures of benzene and ethyl acetate, to give 6.1 g of the desired compound.

후처리

  1. stirringstirred at -20° C. for 15 minutes
  2. additionwas added to the above mixture
  3. stirringstirred at -20° C. for 1 hour
  4. temperatureThe mixture was cooled to -50° C.
  5. extractionThe mixture was extracted with ethyl acetate
  6. washThe extract was washed with a saturated aqueous solution of sodium chloride
  7. dry with materialdried over anhydrous sodium sulphate
  8. distillationThe solvent was distilled off
  9. washeluted with 3:1-2:1 by volume mixtures of benzene and ethyl acetate

출처 및 근거

ORD 기록
ord-fd153148a334471a80be5c976744feec
출처 데이터셋
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04613595

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