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N,N-Dimethylaniline → 7beta-[2-(5-aminomethyl-2-thienyl)-acetylamino]-3-[(1-methyl-1H-tetrazol-5-ylthio)-methyl]-ceph-3-em-4-carboxylic acid

HRID 2398515
ノート
印刷プレビュー

反応式

HRID 2398515 の反応式
C[N:2]([CH3:9])C1C=CC=CC=1.C[Si](C)(C)Cl.NC1C(=O)N2C(C(O)=O)=C([S:24][C:25]3[N:29]([CH3:30])[N:28]=[N:27][N:26]=3)C(C)S[C@H]12.C(OC([NH:43][CH2:44][C:45]1[S:49][C:48]([CH2:50][C:51](Cl)=[O:52])=[CH:47][CH:46]=1)=O)(C)(C)C.C(OC(NC[C:63]1[S:67][C:66]([CH2:68][C:69]([OH:71])=O)=[CH:65][CH:64]=1)=O)(C)(C)C.[C:72](=[O:75])(O)[O-:73].[Na+].C([N:79](CC)CC)C>C(Cl)Cl.O>[NH2:43][CH2:44][C:45]1[S:49][C:48]([CH2:50][C:51]([NH:79][C@@H:68]2[C:69](=[O:71])[N:2]3[C:9]([C:72]([OH:73])=[O:75])=[C:64]([CH2:65][S:24][C:25]4[N:29]([CH3:30])[N:28]=[N:27][N:26]=4)[CH2:63][S:67][C@H:66]23)=[O:52])=[CH:47][CH:46]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 7

HCID 949N,N-DimethylanilineHCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 202932812-[5-({[(Tert-butoxy)carbonyl]amino}methyl)thiophen-2-yl]aceticacidHCID 571344742-(5-Tert.-butoxycarbonylaminomethyl-2-thienyl)-acetic acid chloride
HCID 131710784
7-amino-3-(1-methyl-1H-tetrazol-5-ylthio)-methylceph-3-em-4-carboxylic acid

生成物 1

HCID 706359557beta-[2-(5-aminomethyl-2-thienyl)-acetylamino]-3-[(1-methyl-1H-tetrazol-5-ylthio)-methyl]-ceph-3-em-4-carboxylic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

反応条件

温度
40 °C

実験手順

1.5 ml of triethylamine, 1.6 ml of N,N-dimethylaniline and 2.3 ml of trimethylchlorosilane are added to a suspension of 2.0 g of 7-amino-3-(1-methyl-1H-tetrazol-5-ylthio)-methylceph-3-em-4-carboxylic acid in 60 ml of methylene chloride. The mixture is warmed to 40° C over the course of 20 minutes whilst stirring, and is then cooled to -10° C. A solution of 2-(5-tert.-butoxycarbonylaminomethyl-2-thienyl)-acetic acid chloride in 20 ml of methylene chloride, which has been prepared in the manner described in Example 2 from 1.95 g of 2(5-tert.-butoxycarbonylaminomethyl-2-thienyl)-acetic acid, is then added. The whole is stirred for 2 hours at 0°-25° C and poured into water, the mixture is adjusted to approx. pH 7 with sodium bicarbonate, extracted with methylene chloride and carefully acidified with concentrated hydrochloric acid and the precipitate formed is filtered off. The filter residue is washed with water and dried in vacuo at room temperature. The dried intermediate product is dissolved in 5 ml of trifluoroacetic acid whilst stirring and after 10 minutes the solution is concentrated in vacuo with repeated addition of toluene. The residue is stirred with 50 ml of methanol and filtered and the filtrate is adjusted to approx. pH 6 with triethylamine and left in a refrigerator for 2 hours. Filtration and washing of the filter residue with a little methanol and ether gives 7β-[2-(5-aminomethyl-2-thienyl)-acetylamino]-3-[(1-methyl-1H-tetrazol-5-ylthio)-methyl]-ceph-3-em-4-carboxylic acid; thin layer chromatogram (silica gel; acetonitrile/water, 4:1): Rf = 0.25; ultraviolet absorption spectrum (in 0.01 N aqueous sodium bicarbonate solution): λmax = 242 mμ (ε = 14,100); infrared absorption spectrum (in mineral oil): bands at 3.07μ, 5.64μ, 5.97μ, 6.26μ, 6.64μ etc.

後処理

  1. temperatureis then cooled to -10° C
  2. additionis then added
  3. stirringThe whole is stirred for 2 hours at 0°-25° C
  4. extractionextracted with methylene chloride
  5. customthe precipitate formed
  6. filtrationis filtered off
  7. washThe filter residue is washed with water
  8. customdried in vacuo at room temperature
  9. dissolutionThe dried intermediate product is dissolved in 5 ml of trifluoroacetic acid
  10. stirringwhilst stirring and after 10 minutes the solution
  11. concentrationis concentrated in vacuo
  12. additionaddition of toluene
  13. stirringThe residue is stirred with 50 ml of methanol
  14. filtrationfiltered
  15. filtrationFiltration
  16. washwashing of the filter residue with a little methanol and ether

出典と根拠

ORDレコード
ord-c2f0213219324e46bcf44533b15a65ca
出典データセット
uspto-grants-1977_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04024249

反応ノート

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