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Hydrochloric Acid → HCID 4101679, 화합물

HRID 377697
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HRID 377697 반응식
[C:1]([NH:4][CH2:5][C:6]([OH:8])=O)(=[O:3])[CH3:2].Cl.N[CH2:11][C:12]([NH2:14])=[O:13].C([N:17](CC)CC)C.Cl>O.C(#N)C.O>[C:12]([NH:14][CH2:2][C:1]([NH:4][CH2:5][C:6]([NH2:17])=[O:8])=[O:3])(=[O:13])[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8471Triethylamine2회HCID 10972AcetylglycineHCID 2723639Glycinamide hydrochloride

생성물 1

HCID 4101679HCID 4101679, 화합물수율 60.5%

시약·촉매·용매 2

HCID 962Water용매
HCID 18373917
Acetonitrile--water (1/1)
용매

실험 절차

N-Acetylglycine (5 g, 43 mmole) and 9.5 g (86 mmole) of glycinamide hydrochloride were dissolved in a 150 mL of a mixture of water-acetonitrile (50:50), 8.65 g (86 mmole) of triethylamine (TEA) and 12.6 g (64 mmole) of 1-ethyl-3(3-dimethyl aminopropyl)carbodiimide (EDC) as a coupling reagent were added to the mixture and the mixture was refluxed for 12 hours. The mixture was left to cool at room temperature, the insoluble materials were filtered and the filtrate was evaporated to dryness in vacuum. The residue was recrystallized from a big fraction of acetonitrile to get a mixture of the product with the salt TEA:HCl, the solid crystals were dissolved in distilled water and purified from the salt by a strong cation exchange chromatography (120 plus). The water fractions were collected and the water was removed by lyophilization to get a pure product 4.5 g (26 mmole), yield of 60%.

후처리

  1. additionwere added to the mixture
  2. temperaturethe mixture was refluxed for 12 hours
  3. waitThe mixture was left
  4. filtrationthe insoluble materials were filtered
  5. customthe filtrate was evaporated to dryness in vacuum
  6. customThe residue was recrystallized from a big fraction of acetonitrile
  7. customto get
  8. custompurified from the salt by a strong cation exchange chromatography (120 plus)
  9. customThe water fractions were collected
  10. customthe water was removed by lyophilization

출처 및 근거

ORD 기록
ord-f354761be1ba4dce898223dc130cd73c
출처 데이터셋
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06028102

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