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Methanesulfonic Acid → HCID 88420175, 화합물

HRID 1755868
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HRID 1755868 반응식
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([C:7](=O)[C:8]([NH:10][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:37])[NH:35][OH:36])[N:33]=[C:29]4[N:28]=[C:27]([CH3:38])[CH:26]=2)=[C:16]3[C:20]([OH:22])=[O:21])=[O:9])[N:6]=1.[NH2:40][O:41][CH2:42][C:43]1[N:48]([CH3:49])[C:47](=[O:50])[C:46]([OH:51])=[CH:45][N:44]=1.CS(O)(=O)=O>CC(N(C)C)=O>[NH2:1][C:2]1[S:3][CH:4]=[C:5](/[C:7](=[N:40]/[O:41][CH2:42][C:43]2[N:48]([CH3:49])[C:47](=[O:50])[C:46]([OH:51])=[CH:45][N:44]=2)/[C:8]([NH:10][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:37])[NH:35][OH:36])[N:33]=[C:29]4[N:28]=[C:27]([CH3:38])[CH:26]=2)=[C:16]3[C:20]([OH:22])=[O:21])=[O:9])[N:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6395Methanesulfonic AcidHCID 19917929HCID 19917929, 화합물HCID 86748850HCID 86748850, 화합물

생성물 1

HCID 88420175HCID 88420175, 화합물수율 58.6%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매2회

실험 절차

(6R,7R)-7-(2-Amino-4-thiazoleglyoxylamido)-3-[[[2-(hydroxycarbamoyl)-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 (65 mg) (0.11 mmol) are dissolved in 4 ml of absolute dimethylacetamide. 24 mg (0.14 mmol) of 2-[(aminooxy)methyl]-5-hydroxy-3-methyl-4(3H)-pyrimidinone and 14 mg (0.14 mmol) of methanesulphonic acid are added. After stirring at room temperature for 20 hours the dimethylacetamide is evaporated in a high vacuum and the residue is taken up in water and stirred for 15 minutes in order to precipitate the product completely. The product is filtered off, washed with water and diethyl ether and dried in a high vacuum at room temperature. There are obtained 48 mg of (6R,7R)-7-[(Z)-2-(2-amino-4-thiazolyl)-2-[[(1,6-dihydro-5-hydroxy-1-methyl-6-oxo-2-pyrimidinyl)methoxy]imino]acetamido]-3-[ [[2-(hydroxycarbamoyl)-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 as a beige powder.

후처리

  1. customis evaporated in a high vacuum
  2. customto precipitate the product completely
  3. filtrationThe product is filtered off
  4. washwashed with water and diethyl ether
  5. customdried in a high vacuum at room temperature

출처 및 근거

ORD 기록
ord-b75e03f1f0d943eb8630a48999a9299e
출처 데이터셋
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05438052

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