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Hydrochloric Acid → HCID 70636430, 화합물

HRID 596846
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HRID 596846 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].[C:37]1([Mg]Br)[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1.Cl.[Cr](O)(O)(=O)=O.C(C1CN2C(=O)C[C@H]2SC=1)=O>C(O)(C)C.CC(C)=O.C(OCC)(=O)C.O1CCCC1>[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]([C:17](=[O:18])[C:37]3[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=3)=[CH:15][S:16][C@H:11]12)=[O:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 313Hydrochloric AcidHCID 24425Chromic AcidHCID 88394735HCID 88394735, 화합물HCID 88777142HCID 88777142, 화합물HCID 178418255HCID 178418255, 화합물

생성물 1

HCID 70636430HCID 70636430, 화합물

시약·촉매·용매 4

HCID 180
Acetone
용매
HCID 3776Isopropanol용매
HCID 8028Tetrahydrofuran용매
HCID 8857Ethyl Acetate용매

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온도
-73 °C

실험 절차

To a cooled (-73° C.), stirred solution of 1.04 g. of benzhydryl 7-(2-thienylacetamido)-3-formyl-2-cephem-4-carboxylate and 8 ml. of tetrahydrofuran was added 2.4 ml. of a 2.5 molar phenylmagnesium bromide solution. After stirring the reaction mixture with cooling for four minutes, 8 ml. of 1N.HCl was added, and the reaction mixture was allowed to warm to 0°. Ethyl acetate was added, and the reaction mixture was then washed twice with cold 1 N.HCl, and twice with brine and then dried over anhydrous sodium sulfate. Evaporation in vacuo to dryness gave a residue which was chromatographed on a silica gel column using a toluene-ethyl acetate gradient. This chromatography failed to separate the unreacted starting material (3-formyl-2-cephem ester) and the product cephem secondary carbinol. Combining the fractions off the column and evaporating in vacuo to dryness gave 0.895 g. of a mixture which was dissolved in 50 ml. of acetone and reacted with 0.77 ml. of a 2.26 molar solution of chromic acid. This reaction mixture was allowed to stir for 15 minutes at room temperature after which time 5 ml. of isopropanol was added. After five minutes the reaction mixture was evaporated in vacuo to dryness, and the residue was dissolved in an ethyl acetate/water slurry and then transferred to a separatory funnel with the aid of ethyl acetate. The organic layer was separated and washed with water (4X) and brine (2X) and then dried over anhydrous sodium sulfate. Evaporation in vacuo to dryness and chromatography of the residue thereby obtained on silica using a toluene-ethyl acetate gradient provided 0.213 g. of the 3-formyl-2-cephem starting material and 0.366 g. (41 percent) of the title product which crystallized from methylene chloride hexane as white needles (m.p. 179°-180°):

후처리

  1. stirringAfter stirring the reaction mixture
  2. temperaturewith cooling for four minutes
  3. temperatureto warm to 0°
  4. washthe reaction mixture was then washed twice with cold 1 N
  5. dry with materialHCl, and twice with brine and then dried over anhydrous sodium sulfate
  6. customEvaporation in vacuo to dryness
  7. customgave a residue which
  8. customwas chromatographed on a silica gel column
  9. customto separate the unreacted starting material (3-formyl-2-cephem ester)
  10. customevaporating in vacuo to dryness
  11. customgave 0.895 g
  12. dissolutionof a mixture which was dissolved in 50 ml
  13. stirringto stir for 15 minutes at room temperature after which time 5 ml
  14. customAfter five minutes the reaction mixture was evaporated in vacuo to dryness
  15. dissolutionthe residue was dissolved in an ethyl acetate/water slurry
  16. customtransferred to a separatory funnel with the aid of ethyl acetate
  17. customThe organic layer was separated
  18. washwashed with water (4X) and brine (2X)
  19. dry with materialdried over anhydrous sodium sulfate
  20. customEvaporation in vacuo to dryness and chromatography of the residue
  21. customthereby obtained on silica using a toluene-ethyl acetate gradient
  22. customprovided 0.213 g
  23. custom(41 percent) of the title product which crystallized from methylene chloride hexane as white needles (m.p. 179°-180°)

출처 및 근거

ORD 기록
ord-365ecef09f9844e597f011ec18c63c77
출처 데이터셋
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04012380

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