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Sodium Bicarbonate → 7-[2-methoxyimino-2-(2,3-dihydro-1,4-dithiin-5-yl)acetamido]-3-(1-carboxymethyl-1H-tetrazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid

HRID 648401
ノート
印刷プレビュー

反応式

HRID 648401 の反応式
[CH3:1][O:2][N:3]=[C:4]([C:8]1[S:9][CH2:10][CH2:11][S:12][CH:13]=1)[C:5]([OH:7])=O.[NH2:14][CH:15]1[C:36](=[O:37])[N:17]2[C:18]([C:33]([OH:35])=[O:34])=[C:19]([CH2:22][S:23][C:24]3[N:28]([CH2:29][C:30]([OH:32])=[O:31])[N:27]=[N:26][N:25]=3)[CH2:20][S:21][C@H:16]12.C(=O)(O)[O-].[Na+]>O.C(OCC)(=O)C.CC(C)=O>[CH3:1][O:2][N:3]=[C:4]([C:8]1[S:9][CH2:10][CH2:11][S:12][CH:13]=1)[C:5]([NH:14][CH:15]1[C:36](=[O:37])[N:17]2[C:18]([C:33]([OH:35])=[O:34])=[C:19]([CH2:22][S:23][C:24]3[N:28]([CH2:29][C:30]([OH:32])=[O:31])[N:27]=[N:26][N:25]=3)[CH2:20][S:21][C@H:16]12)=[O:7]
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 3

HCID 516892Sodium Bicarbonate2 回HCID 127691497-amino-3-(1-carboxymethyl-1H-tetrazol-5-yl)thiomethyl-3-cephem-4-carboxylic acidHCID 539358522-Methoxyimino-2-(2,3-dihydro-1,4-dithiin-5-yl)acetic acid

生成物 1

HCID 1317124017-[2-methoxyimino-2-(2,3-dihydro-1,4-dithiin-5-yl)acetamido]-3-(1-carboxymethyl-1H-tetrazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid収率 78%

試薬・触媒・溶媒 3

HCID 180Acetone溶媒
HCID 962Water溶媒
HCID 8857Ethyl Acetate溶媒2 回

実験手順

Ethyl acetate (15 ml.) and 2-methoxyimino-2-(2,3-dihydro-1,4-dithiin-5-yl)acetic acid (syn isomer) (2.0 g.) were added to the solution at -10° C. to give a solution. On the other hand, a suspension of 7-amino-3-(1-carboxymethyl-1H-tetrazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid (2.83 g.) in water (40 ml.) was changed to a solution by adding sodium bicarbonate (1.45 g.), and then acetone (40 ml.) was added thereto. After the solution was adjusted to pH7.3, the ethyl acetate solution obtained above was added dropwise thereto over 10 minutes with stirring at -5° to -7° C., during which the pH of the mixture was kept at 6.8 to 7.3 with an aqueous solution of sodium bicarbonate. The mixture was stirred for 1.5 hours at the same temperature. The resultant solution was adjusted to pH7.8 and washed with ethyl acetate (40 ml.). The solution was adjusted to pH6 and washed with ethyl acetate (40 ml.). And the solution was adjusted to pH2 and extracted with ethyl acetate (100 ml.). The extract was washed with a saturated aqueous solution of sodium chloride (60 ml.) and dried over magnesium sulfate. The extract was concentrated in vacuo, and the residue was washed with diethyl ether and collected by filtration to give pale yellow crystals of 7-[2-methoxyimino-2-(2,3-dihydro-1,4-dithiin-5-yl)acetamido]-3-(1-carboxymethyl-1H-tetrazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid (syn isomer) (3.4 g.).

後処理

  1. customto give a solution
  2. additionabove was added dropwise
  3. stirringThe mixture was stirred for 1.5 hours at the same temperature
  4. washwashed with ethyl acetate (40 ml.)
  5. washwashed with ethyl acetate (40 ml.)
  6. extractionextracted with ethyl acetate (100 ml.)
  7. washThe extract was washed with a saturated aqueous solution of sodium chloride (60 ml.)
  8. dry with materialdried over magnesium sulfate
  9. concentrationThe extract was concentrated in vacuo
  10. washthe residue was washed with diethyl ether
  11. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-abed65756a6d489480ea5a5309908107
出典データセット
uspto-grants-1983_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04411898

反応ノート

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