Cyanoacetic acid → HCID 2799775、化合物

HRID 566252ノート

反応式

HRID 566252 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 2799775HCID 2799775、化合物収率 88.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b94eb658116f456090fdb6f236f27fa3
出典データセット
uspto-grants-2001_01
特許番号
US06174877B1

反応ノート

読み込み中…