1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 86743292, 화합물

HRID 1722632노트

반응식

HRID 1722632 반응식
[C:1]([O:5][C:6]([N:8]1[CH:12]=[C:11]([CH2:13][C:14]([OH:16])=O)[N:10]=[CH:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH2:17][CH:18]([P:27](=[O:34])([O:31][CH2:32][CH3:33])[O:28][CH2:29][CH3:30])[P:19](=[O:26])([O:23][CH2:24][CH3:25])[O:20][CH2:21][CH3:22].Cl.C(N=C=NCCCN(C)C)C>CN(C)C=O.C(Cl)(Cl)Cl>[C:1]([O:5][C:6]([N:8]1[CH:12]=[C:11]([CH2:13][C:14]([NH:17][CH:18]([P:19](=[O:26])([O:20][CH2:21][CH3:22])[O:23][CH2:24][CH3:25])[P:27](=[O:34])([O:31][CH2:32][CH3:33])[O:28][CH2:29][CH3:30])=[O:16])[N:10]=[CH:9]1)=[O:7])([CH3:2])([CH3:3])[CH3:4]

참가 물질

6

반응물 3

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 2773808Tetraethyl aminomethylenediphosphonateHCID 22161426HCID 22161426, 화합물

생성물 1

HCID 86743292HCID 86743292, 화합물수율 65.9%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of 2-[1-(tert-butoxycarbonyl)imidazol-4-yl]acetic acid (45 mg) and tetraethyl (aminomethylene)bis(phosphonate) (91 mg) in N,N-dimethylformamide (1 ml) was added N-ethyl-N'-(3-dimethylaminopropyl)carbodiimide hydrochloride (42 mg) with stirring on ice-sodium chloride bath under nitrogen atmosphere. After stirring for 36 hours at 5° C., the mixture was diluted with chloroform (10 ml) and washed with cold 1N aqueous solution of citric acid (10 ml). The aqueous layer was extracted with chloroform (10 ml) twice and the combined organic layers were dried over sodium sulfate and evaporated in vacuo. The residue was dissolved in ethyl acetate (10 ml) and the solution was washed with water (10 ml), dried over sodium sulfate and evaporated in vacuo to give a colorless syrup of tetraethyl [[2-{1-(tert-butoxycarbonyl)imidazol-4-yl}acetamido]methylene]bis(phosphonate) (67 mg).

후처리

  1. stirringAfter stirring for 36 hours at 5° C.
  2. washwashed with cold 1N aqueous solution of citric acid (10 ml)
  3. extractionThe aqueous layer was extracted with chloroform (10 ml) twice
  4. dry with materialthe combined organic layers were dried over sodium sulfate
  5. customevaporated in vacuo
  6. dissolutionThe residue was dissolved in ethyl acetate (10 ml)
  7. washthe solution was washed with water (10 ml)
  8. dry with materialdried over sodium sulfate
  9. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-6bee08c902aa40d9a0a7e50a61c8a631
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04857513

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