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Pyridine → Benzhydryl 7-amino-3-acetyl-2-cephem-4-carboxylate

HRID 596838
ノート
印刷プレビュー

反応式

HRID 596838 の反応式
P(Cl)(Cl)(Cl)(Cl)Cl.S1C=CC=C1CC([NH:15][CH:16]1[C:42](=[O:43])[N:18]2[CH:19]([C:26]([O:28][CH:29]([C:36]3[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=3)[C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)=[O:27])[C:20]([C:23](=[O:25])[CH3:24])=[CH:21][S:22][C@H:17]12)=O.N1C=CC=CC=1.C(Cl)Cl>CCCCCC.C(O)C(C)C>[NH2:15][CH:16]1[C:42](=[O:43])[N:18]2[CH:19]([C:26]([O:28][CH:29]([C:36]3[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=3)[C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)=[O:27])[C:20]([C:23](=[O:25])[CH3:24])=[CH:21][S:22][C@H:17]12
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 1049PyridineHCID 6344DichloromethaneHCID 24819Phosphorus pentachlorideHCID 70636001Benzhydryl 7-(2-thienylacetamido)-3-acetyl-2-cephem-4-carboxylate

生成物 1

HCID 131710673Benzhydryl 7-amino-3-acetyl-2-cephem-4-carboxylate収率 64%

試薬・触媒・溶媒 2

HCID 6560
Isobutanol
溶媒
HCID 8058Hexane溶媒

実験手順

Phosphorous pentachloride (0.478 g.) was added to a stirred solution of 1.065 g. of benzhydryl 7-(2-thienylacetamido)-3-acetyl-2-cephem-4-carboxylate and 0.199 ml. of pyridine in 9 ml. of methylene chloride. The reaction mixture was allowed to stir at room temperature for 2.5 hours. After cooling the mixture for 5 minutes in an ice bath, 0.985 ml. of isobutanol was added, and the reaction mixture was subsequently stirred at room temperature for one hour. The addition of n-hexane resulted in the formation of a brown solid from which the liquid was decanted. The residue was dissolved in an ethyl acetate-aqueous sodium bicarbonate slurry and transferred to a separatory funnel with the aid of ethyl acetate. The organic layer was separated and washed successively with aqueous sodium bicarbonate solution, water, and brine (2X), and dried over anhydrous sodium sulfate. Evaporation in vacuo to dryness provided a product which was chromatographed on a silica gel column using a toluene-ethyl acetate gradient to give a 0.521 g. (64 percent) of the title product as a tan froth:

後処理

  1. temperatureAfter cooling the mixture for 5 minutes in an ice bath
  2. stirringthe reaction mixture was subsequently stirred at room temperature for one hour
  3. customresulted in the formation of a brown solid from which the liquid
  4. customwas decanted
  5. dissolutionThe residue was dissolved in an ethyl acetate-aqueous sodium bicarbonate slurry
  6. customtransferred to a separatory funnel with the aid of ethyl acetate
  7. customThe organic layer was separated
  8. washwashed successively with aqueous sodium bicarbonate solution, water, and brine (2X)
  9. dry with materialdried over anhydrous sodium sulfate
  10. customEvaporation in vacuo to dryness
  11. customprovided a product which
  12. customwas chromatographed on a silica gel column
  13. customto give a 0.521 g

出典と根拠

ORDレコード
ord-632e4774818046028ab902c67241b186
出典データセット
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04012380

反応ノート

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