Hydrochloric Acid → HCID 178419078、化合物

HRID 1731194

反応式

HRID 1731194 の反応式
NCC([NH:5][C@H:6]([C:13]([OH:15])=[O:14])[CH2:7][C:8]1[N:12]=[CH:11][NH:10][CH:9]=1)=O.C(SC(=N)N)C.OS(O)(=O)=O.[NH2:27]CC(N[C@H](C(O)=O)CC1N=CNC=1)=O.Cl.[OH-:43].[Na+].C(C(O)(C([O-])=O)CC([O-])=O)C([O-])=O.C(C(O)(C([O-])=O)CC([O-])=O)C([O-])=O.[OH2:71].[Na+].[Na+].[Na+].[K+].[K+].[K+].C1C=C2C(C(O)(O)C(=O)C2=CC=1)=O.N(CC(N[C@H](C(O)=O)CC1N=CNC=1)=O)C(N)=N.Cl>O.N1C=CC=CC=1>[NH:12]([CH2:8][C:9]([OH:71])=[O:43])[C:11]([NH2:10])=[NH:27].[NH2:5][C@H:6]([C:13]([OH:15])=[O:14])[CH2:7][C:8]1[N:12]=[CH:11][NH:10][CH:9]=1

参加物

13

反応物 9

HCID 313Hydrochloric AcidHCID 1118Sulfuric Acid2 回HCID 5139S-Ethylisothiourea2 回HCID 10236NinhydrinHCID 14798Sodium HydroxideHCID 171403Sodium citrate, potassium citrate, citric acidHCID 178479243HCID 178479243、化合物HCID 178511447HCID 178511447、化合物HCID 178513020HCID 178513020、化合物

生成物 2

HCID 178419078HCID 178419078、化合物HCID 178513022HCID 178513022、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒4 回HCID 1049Pyridine溶媒4 回

実験手順

H2O (n=1) was prepared from glycyl-L-histidine and S-ethylisothiourea.H2SO4. Solutions of 1.50 g. of S-ethylisothiourea.H2SO4 in 5 ml of H2O and 1.74 g. of Gly-His.HCl in 3 ml of H2O were adjusted to pH 8-9 with 4 N NaOH. They were then mixed and kept at room temperature for a week. The cloudy suspension was filtered and the filtrate concentrated to dryness in vacuo. The residue, after addition of a small amount of EtOH, was dried in vacuo. A small amount of H2O was added to dissolve the dry residue and resulting solution was poured onto the column (2.5 cm i.d. × 30 cm Amberlite CG-120, 200-400 mesh, pyridine form). H2O, 1.0 M pyridine, 2.0 M pyridine, and 1.0 M pyridine--0.5 M NH4OH were used as the effluent solutions. Each fraction was tested for ninhydrin, Pauli, and Sakaguchi reactions. The fractions containing guanidinoacetyl-L-histidine were pooled and concentrated to dryness in vacuo. Cryst from H2O--EtOH; yield, 69.2%; mp, 108-111° C., decomp. Hydrolysis (6 N HCl, 110° , 24 hours.) gave guanidinoacetic acid and histidine, as confirmed be tlc. (thin layer chromatography).

後処理

  1. additionThey were then mixed
  2. waitkept at room temperature for a week
  3. filtrationThe cloudy suspension was filtered
  4. concentrationthe filtrate concentrated to dryness in vacuo
  5. additionThe residue, after addition of a small amount of EtOH
  6. customwas dried in vacuo
  7. additionA small amount of H2O was added
  8. dissolutionto dissolve the dry residue
  9. customresulting solution
  10. concentrationconcentrated to dryness in vacuo
  11. customyield

出典と根拠

ORDレコード
ord-f481a805934f4387a2abd702b14ad33c
出典データセット
uspto-grants-1976_11
特許番号
US03995051

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