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Hydrochloric Acid → HCID 70636145, 화합물

HRID 596843
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HRID 596843 반응식
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][C:7]([NH:9][CH:10]1[C:35](=[O:36])[N:12]2[CH:13]([C:19]([O:21][CH:22]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)[C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)=[O:20])[C:14]([CH:17]=[O:18])=[CH:15][S:16][C@H:11]12)=[O:8].O1CC[CH2:39][CH2:38]1.C([Mg]Br)C.Cl>C(OCC)(=O)C>[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][C:7]([NH:9][CH:10]1[C:35](=[O:36])[N:12]2[CH:13]([C:19]([O:21][CH:22]([C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=3)[C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[O:20])[C:14]([CH:17]([OH:18])[CH2:38][CH3:39])=[CH:15][S:16][C@H:11]12)=[O:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric Acid2회HCID 8028TetrahydrofuranHCID 88777142HCID 88777142, 화합물HCID 178418443HCID 178418443, 화합물

생성물 1

HCID 70636145HCID 70636145, 화합물수율 30.6%

시약·촉매·용매 1

HCID 8857Ethyl Acetate
용매

반응 조건

온도
-73 °C

실험 절차

To a cooled (-73° C.), stirred solution of 1.559 g. of benzhydryl 7-(2-thienylacetamido)-3-formyl-2-cephem-4-carboxylate and 20 ml. of dry tetrahydrofuran was added 3.13 ml. of 2.88 M. ethyl magnesium bromide. After the reaction mixture was allowed to stir for four minutes at -73° C., 10 ml. of 1N.HCl was added and the solution allowed to warm to 0° C. The reaction mixture was transferred to a separatory funnel with the aid of cold ethyl acetate and cold 1N.HCl. The organic layer was separated and washed twice with cold 1N.HCl and twice with brine and then dried over anhydrous sodium sulfate. Evaporation in vacuo to dryness provided a product residue which was chromatographed on silica gel using a toluene-ethyl acetate gradient to give 0.140 g. of the starting 3-formyl-2-cephem ester and 0.507 g. (30.6 percent) of the title product as a mixture of diasteromers:

후처리

  1. stirringto stir for four minutes at -73° C.
  2. temperatureto warm to 0° C
  3. customThe organic layer was separated
  4. washwashed twice with cold 1N
  5. dry with materialHCl and twice with brine and then dried over anhydrous sodium sulfate
  6. customEvaporation in vacuo to dryness
  7. customprovided a product residue which
  8. customwas chromatographed on silica gel using a toluene-ethyl acetate gradient
  9. customto give 0.140 g

출처 및 근거

ORD 기록
ord-e4f5ddd6e0e34fef81046c8671477ac0
출처 데이터셋
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04012380

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