Cyanoacetic acid → HCID 2799775, 화합물

HRID 566252노트

반응식

HRID 566252 반응식
[C:1]([CH2:3][C:4]([OH:6])=O)#[N:2].[NH2:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1.Cl.C(N=C=NCCCN(C)C)C.C(=O)([O-])O.[Na+]>ClCCl>[C:1]([CH2:3][C:4]([NH:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1)=[O:6])#[N:2]

참가 물질

6

반응물 4

HCID 9740Cyanoacetic acidHCID 195092-PyridinemethanamineHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

생성물 1

HCID 2799775HCID 2799775, 화합물수율 88.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Cyanoacetic acid (8.51 g) was dissolved in dichloromethane (400 ml). To the solution was added 2-aminomethylpyridine (10.81 g). The mixture was stirred for a while, to which was then added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (19.17 g). The mixture was stirred for 15 minutes at 25° C. To the reaction mixture was added a saturated aqueous solution of sodium hydrogencarbonate (200 ml). The mixture was shaken and left standing. The.aqueous layer was subjected to extraction with ethyl acetate (200 ml) three times. The organic layers were combined and dried over anhydrous magnesium sulfate, followed by concentration to afford the title compound (15.51 g).

후처리

  1. stirringThe mixture was stirred for 15 minutes at 25° C
  2. stirringThe mixture was shaken
  3. waitleft standing
  4. extractionThe.aqueous layer was subjected to extraction with ethyl acetate (200 ml) three times
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationfollowed by concentration

출처 및 근거

ORD 기록
ord-b94eb658116f456090fdb6f236f27fa3
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06174877B1

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