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7-Aminocephalosporanic acid → 7-Amino-3-(4,6-diamino-pyrimidin-2-yl-thiomethyl)-ceph-3-em-4-carboxylic acid dihydrate

HRID 1534457
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HRID 1534457 반응식
CC(O[CH2:5][C:6]1[CH2:15][S:14][C@@H:9]2[C@H:10]([NH2:13])[C:11](=[O:12])[N:8]2[C:7]=1[C:16]([OH:18])=[O:17])=[O:3].[NH2:19][C:20]1[CH:25]=[C:24]([NH2:26])[N:23]=[C:22]([SH:27])[N:21]=1>O.C(=O)(O)[O-].[Na+]>[OH2:3].[OH2:3].[NH2:13][CH:10]1[C:11](=[O:12])[N:8]2[C:7]([C:16]([OH:18])=[O:17])=[C:6]([CH2:5][S:27][C:22]3[N:23]=[C:24]([NH2:26])[CH:25]=[C:20]([NH2:19])[N:21]=3)[CH2:15][S:14][C@H:9]12
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참가 물질

5

반응물 2

HCID 4413287-Aminocephalosporanic acidHCID 1785079174,6-diaminopyrimidine-2-thiol

생성물 1

HCID 676616387-Amino-3-(4,6-diamino-pyrimidin-2-yl-thiomethyl)-ceph-3-em-4-carboxylic acid dihydrate수율 82.5%

시약·촉매·용매 2

HCID 962Water용매HCID 516892Sodium Bicarbonate용매2회

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온도
60 °C

실험 절차

2.7 g (0.01 mole) of 7-aminocephalosporanic acid are dissolved in 50 ml of water with the required amount of sodium bicarbonate. 1.7 g (0.013 mole) of 4,6-diamino-2-mercapto-pyrimidine and the equivalent amount of sodium bicarbonate are added and the reaction solution is heated to 60° C. for 4 hours, whilst stirring and keeping the pH value constant (pH=7). The mixture is allowed to cool, undissolved material is filtered off and the filtrate is concentrated in vacuo at 30° C. to half its volume. The aqueous solution which remains is extracted several times with ethyl acetate and the aqueous phase is adjusted to a pH of 2 with 2N hydrochloric acid. The precipitate is filtered off, washed with water until free from chloride and dried in vacuo at 37° C. over potassium hydroxide. 1.61 g of the title compound are obtained.

후처리

  1. temperatureto cool
  2. filtrationundissolved material is filtered off
  3. concentrationthe filtrate is concentrated in vacuo at 30° C. to half its volume
  4. extractionThe aqueous solution which remains is extracted several times with ethyl acetate
  5. filtrationThe precipitate is filtered off
  6. washwashed with water until free from chloride
  7. dry with materialdried in vacuo at 37° C. over potassium hydroxide

출처 및 근거

ORD 기록
ord-d927bad9c44441cd803cf247a0d28a9f
출처 데이터셋
uspto-grants-1992_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05089490

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