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Sodium → 3-[(Acetyloxy)methyl]-7-[[(2-formyl-1-pyrryl)acetyl]amino]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid N-ethoxycarbonyl-N-methylaminomethyl ester

HRID 1448575
ノート
印刷プレビュー

反応式

HRID 1448575 の反応式
[Na].[C:2]([O:5][CH2:6][C:7]1[CH2:14][S:13][CH:12]2[N:9]([C:10](=[O:26])[CH:11]2[NH:15][C:16](=[O:25])[CH2:17][N:18]2[CH:22]=[CH:21][CH:20]=[C:19]2[CH:23]=[O:24])[C:8]=1[C:27]([OH:29])=[O:28])(=[O:4])[CH3:3].Cl[CH2:31][N:32]([CH3:38])[C:33]([O:35][CH2:36][CH3:37])=[O:34]>CN(C)C=O>[CH2:36]([O:35][C:33]([N:32]([CH2:38][O:28][C:27]([C:8]1[N:9]2[CH:12]([S:13][CH2:14][C:7]=1[CH2:6][O:5][C:2](=[O:4])[CH3:3])[CH:11]([NH:15][C:16](=[O:25])[CH2:17][N:18]1[CH:22]=[CH:21][CH:20]=[C:19]1[CH:23]=[O:24])[C:10]2=[O:26])=[O:29])[CH3:31])=[O:34])[CH3:37]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 5360545SodiumHCID 15790124Ethyl N-(chloromethyl)-N-methylcarbamateHCID 867361063-[(Acetyloxy)methyl]-7-[[(2-formyl-1-pyrryl)acetyl]amino]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid

生成物 1

HCID 867361093-[(Acetyloxy)methyl]-7-[[(2-formyl-1-pyrryl)acetyl]amino]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid N-ethoxycarbonyl-N-methylaminomethyl ester

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

The sodium salt of 3-[(acetyloxy)methyl]-7-[[(2-formyl-1-pyrryl)acetyl]amino]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid (2.5 mmole) in 50 ml of dimethylformamide (DMF) is treated at room temperature with 2.5 mmole of N-chloromethyl-N-methylurethane for 1 hour. The mixture is carefully poured into ice water and the precipitated solid is removed by filtration and is then washed with water. The filtered solid is dissolved in ethyl acetate and washed with aqueous sodium bicarbonate and then with water. The organic layer is dried over magnesium sulfate, filtered and evaporated to dryness to give the title compound.

後処理

  1. customthe precipitated solid is removed by filtration
  2. washis then washed with water
  3. dissolutionThe filtered solid is dissolved in ethyl acetate
  4. washwashed with aqueous sodium bicarbonate
  5. dry with materialThe organic layer is dried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-b915c94ebfc14b64bc8728fac28fb6e2
出典データセット
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04180660

反応ノート

読み込み中…

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