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Hydrochloric Acid → HCID 70436365、化合物

HRID 256100
ノート
印刷プレビュー

反応式

HRID 256100 の反応式
[O:1]([CH2:8][C:9]([NH:11][C@@H:12]1[C:50](=[O:51])[N:14]2[C:15]([C:34]([O:36][CH:37]([C:44]3[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=3)[C:38]3[CH:43]=CC=[CH:40][CH:39]=3)=[O:35])=[C:16](OP(C3C=CC=CC=3)(C3C=CC=CC=3)=O)[CH2:17][S:18][C@H:13]12)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[SH-:52].[Na+].[C:54]([O:58][CH2:59][CH:60]=[CH2:61])(=[O:57])[C:55]#[CH:56].Cl.C(N([CH:69]([CH3:71])C)CC)(C)C>CN(C)C=O>[O:1]([CH2:8][C:9]([NH:11][C@@H:12]1[C:50](=[O:51])[N:14]2[C:15]([C:34]([O:36][CH:37]([C:44]3[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=3)[C:38]3[CH:43]=[CH:71][CH:69]=[CH:40][CH:39]=3)=[O:35])=[C:16]([S:52]/[CH:56]=[CH:55]\[C:54]([O:58][CH2:59][CH:60]=[CH2:61])=[O:57])[CH2:17][S:18][C@H:13]12)=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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 5

HCID 313Hydrochloric AcidHCID 28015Sodium hydrosulfideHCID 81531DiisopropylethylamineHCID 84443Propiolic acid, allyl esterHCID 14535654HCID 14535654、化合物

生成物 1

HCID 70436365HCID 70436365、化合物収率 61%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a cooled (-10° C.) solution of 1.5 g (2 mM) of benzhydryl 7β-phenoxyacetamido-3-diphenylphosphoryloxy-3-cephem-4-carboxylate in 12 ml of N,N-dimethylformamide were added a solution of 177 mg (2.2 mM) of 70% sodium hydrosulfide in 8 ml of N,N-dimethylformamide and 310 mg (2.4 mM) of diisopropylethylamine, and the reaction mixture was stirred for 30 minutes. Subsequently, 330 mg (3 mM) of allyl propiolate was added at the same temperature, and the reaction mixture was stirred for 40 minutes. After the reaction, 50 ml of 0.5% hydrochloric acid was added, the mixture was extracted with 100 ml of ethyl acetate, and the extract was washed with a saturated aqueous sodium chloride solution (100 ml×2) and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the residue was purified by silica gel column chromatography (eluent; ethyl acetate : n-hexane=2 : 3 to 1 : 1) to give 820 mg of benzhydryl 7β-phenoxyacetamido-3-[(Z)-2allyloxycarbonylvinylthio]-3-cephem-4-carboxylate.

後処理

  1. stirringthe reaction mixture was stirred for 40 minutes
  2. additionwas added
  3. extractionthe mixture was extracted with 100 ml of ethyl acetate
  4. washthe extract was washed with a saturated aqueous sodium chloride solution (100 ml×2)
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated
  7. customthe residue was purified by silica gel column chromatography (eluent; ethyl acetate : n-hexane=2 : 3 to 1 : 1)

出典と根拠

ORDレコード
ord-c2dd6548fc734343bd77b36ef5df2df4
出典データセット
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04699981

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート