Water → Benzyl(cyano)methylamine

HRID 1646556노트

반응식

HRID 1646556 반응식
[CH3:1][N:2]([CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:3]([NH2:5])=O.C(N(CC)CC)C.O>C(Cl)(Cl)Cl.[OH-].[Na+]>[CH3:1][N:2]([CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:3]#[N:5]

참가 물질

6

반응물 3

HCID 962WaterHCID 8471TriethylamineHCID 156760161-benzyl-1-methylurea

생성물 1

HCID 12526219Benzyl(cyano)methylamine수율 82.1%

시약·촉매·용매 2

HCID 6212Chloroform용매2회HCID 14798Sodium Hydroxide용매

실험 절차

To N-methyl-N-benzylurea (1.64 g, 0.01 mol) in chloroform (24 ml) and 50% aqueous sodium hydroxide solution (5.4 ml) was added triethylamine (0.1 g, 0.001 mol) and the mixture was vigorously stirred at room temperature for 3.5 h. After addition of water and chloroform, the mixture was stirred, then extracted with chloroform. The extracts were washed with water, dried with anhydrous sodium sulfate, and evaporated under reduced pressure to a residue, which was chromatographed to afford N-methyl-N-benzylcyanamide (1.2 g, 82% yield) as oily substance: NMR(CDCl3)δ2.77(s, 3H), 4.14(s, 2H), 7.25-7.50(m, 5H); IR(neat) 220, 1495, 1455, 1365, 730 cm-1.

후처리

  1. stirringthe mixture was stirred
  2. extractionextracted with chloroform
  3. washThe extracts were washed with water
  4. dry with materialdried with anhydrous sodium sulfate
  5. customevaporated under reduced pressure to a residue, which
  6. customwas chromatographed

출처 및 근거

ORD 기록
ord-561ca7d234064ef7a48c98aa6e719ad8
출처 데이터셋
uspto-grants-1993_01
특허 번호
US05180731

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