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Hydrochloric Acid → (5-Methyl-2-oxo-1,3-dioxolen-4-yl)methyl 7-formamido-3-(1,2,4-thiadiazol-4-yl)thiomethyl-3-cephem-4-carboxylate

HRID 34268
ノート
印刷プレビュー

反応式

HRID 34268 の反応式
[CH:1]([NH:3][CH:4]1[C:21](=[O:22])[N:6]2[C:7]([C:18]([OH:20])=[O:19])=[C:8]([CH2:11][S:12][N:13]3[CH2:17][S:16][N:15]=[CH:14]3)[CH2:9][S:10][C@H:5]12)=[O:2].[CH2:23]1OC1C.Br[C:28]1[O:29][C:30](=[O:35])[O:31][C:32]=1[CH2:33]C.Cl>CN(C=O)C.CCOC(C)=O>[CH:1]([NH:3][CH:4]1[C:21](=[O:22])[N:6]2[C:7]([C:18]([O:20][CH2:23][C:28]3[O:29][C:30](=[O:35])[O:31][C:32]=3[CH3:33])=[O:19])=[C:8]([CH2:11][S:12][N:13]3[CH2:17][S:16][N:15]=[CH:14]3)[CH2:9][S:10][C@H:5]12)=[O:2]
参加物反応条件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 313Hydrochloric AcidHCID 6378Propylene OxideHCID 704066334-Bromo-methyl-5-methyl-1,3-dioxolene-2-oneHCID 886407317-Formamido-3-(1,2,4-thiadiazol-4-yl)thiomethyl-3-cephem-4-carboxylic acid

生成物 1

HCID 131715666(5-Methyl-2-oxo-1,3-dioxolen-4-yl)methyl 7-formamido-3-(1,2,4-thiadiazol-4-yl)thiomethyl-3-cephem-4-carboxylate

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
5 °C

実験手順

A suspension of 7-formamido-3-(1,2,4-thiadiazol-4-yl)thiomethyl-3-cephem-4-carboxylic acid (1.07 g, 3 mmole), KHCO3 (1.0 g, 10 mmole) and propylene oxide (1 ml) in DMF (5 ml) was cooled to 5° C. and treated with 4-bromo-methyl-5-methyl-1,3-dioxolene-2-one (0.87 g, 4.5 mmole). After stirring at 5° C. for 5 hr, the reaction mixture was poured into a mixture of aq HCl (pH 3) (70 ml) and EtOAc (250 ml). The EtOAc layer was separated and washed successively with aq HCl (pH 3) (70 ml×2), 10% K2HPO4 buffer (pH 7) (70 ml×2) and saturated aq NaCl (50 ml). The EtOAc solution was dried (MgSO4) and concentrated in vacuo. The residue was triturated with ether (300 ml) and the resulting precipitate was filtered to give the title compound ( 0.45 g).

後処理

  1. customThe EtOAc layer was separated
  2. washwashed successively with aq HCl (pH 3) (70 ml×2), 10% K2HPO4 buffer (pH 7) (70 ml×2) and saturated aq NaCl (50 ml)
  3. dry with materialThe EtOAc solution was dried (MgSO4)
  4. concentrationconcentrated in vacuo
  5. customThe residue was triturated with ether (300 ml)
  6. filtrationthe resulting precipitate was filtered

出典と根拠

ORDレコード
ord-be25827142204a54ba9cfb56b41c74fe
出典データセット
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04761409

反応ノート

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