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p-Toluenesulfonic acid monohydrate → 3-[[[2-Carbamoyl-5-methyl-s-triazolo[1,5-a]-pyrimidin-7-yl) thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid

HRID 345172
ノート
印刷プレビュー

反応式

HRID 345172 の反応式
NC1SC=C(C(=O)C(N[C@@H:11]2[C:18](=[O:19])[N:17]3[C@@H:12]2[S:13][CH2:14][C:15]([CH2:23][S:24][C:25]2[N:30]4[N:31]=[C:32]([C:34](=[O:36])[NH2:35])[N:33]=[C:29]4[N:28]=[C:27]([CH3:37])[CH:26]=2)=[C:16]3[C:20]([OH:22])=[O:21])=O)N=1.NOC(C)(C)C(NNC(C1NC=C(O)C(=O)C=1)=O)=O.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CC(N(C)C)=O>[C:34]([C:32]1[N:33]=[C:29]2[N:28]=[C:27]([CH3:37])[CH:26]=[C:25]([S:24][CH2:23][C:15]3[CH2:14][S:13][CH:12]4[N:17]([C:18](=[O:19])[CH2:11]4)[C:16]=3[C:20]([OH:22])=[O:21])[N:30]2[N:31]=1)(=[O:36])[NH2:35]
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 521998p-Toluenesulfonic acid monohydrateHCID 199939031-[2-(Aminooxy)-2-methylpropionyl]-2-[(1,4-dihydro-5-hydroxy-4-oxo-2-pyridyl)carbonyl]hydrazineHCID 86744944(6R,7R)-7-(2-amino-4-thiazoleglyoxylamido)-3-[[(2-carbamoyl-5-methyl-s-triazolo[1,5-a]pyrimidin-7-yl)thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid

生成物 1

HCID 199939003-[[[2-Carbamoyl-5-methyl-s-triazolo[1,5-a]-pyrimidin-7-yl) thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒2 回

実験手順

0.228 g (0.4 mmol) of (6R,7R)-7-(2-amino-4-thiazoleglyoxylamido)-3-[[(2-carbamoyl -5-methyl-s-triazolo[1,5-a]pyrimidin-7-yl)thio]methyl]-8-oxo-5-thia-1-azabicyclo [4.2.0]oct-2-ene-2-carboxylic acid was dissolved in 2 ml of dimethylacetamide. 0.140 g (0.52 mmol) of 1-[2-(aminooxy)-2-methylpropionyl]-2-[(1,4-dihydro-5-hydroxy-4-oxo-2-pyridyl) carbonyl]hydrazine and 0.100 g (0.52 mmol) of p-toluenesulfonic acid hydrate were added. After stirring for 20 hours at room temperature the dimethylacetamide was evaporated off at strongly reduced pressure and the residue was taken up in water and stirred for 15 minutes in order to completely precipitate the product. The product was filtered off, washed well with water and dried under strongly reduced pressure at room temperature. (6R,7R)-7-[(Z)-2-(2-amino-4-thiazolyl)-2-[[1,4-dihydro-5-hydroxy -4-oxo-2-pyridyl)carbonyl]carbazoyl]-1-methylethoxy]imino] -acetamido]-3-[[[2-carbamoyl-5-methyl-s-triazolo[1,5-a]-pyrimidin-7-yl) thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid was obtained as beige-colored powder.

後処理

  1. customwas evaporated off at strongly reduced pressure
  2. customto completely precipitate the product
  3. filtrationThe product was filtered off
  4. washwashed well with water
  5. customdried under strongly reduced pressure at room temperature

出典と根拠

ORDレコード
ord-0957e77b73c54ee08d23b4631afce85a
出典データセット
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05055572

反応ノート

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