Water → N-{2-[6-(cyanomethyl)-1,3-benzodioxol-5-yl]ethyl}acetamide

HRID 462098노트

반응식

HRID 462098 반응식
Cl[CH2:2][C:3]1[C:8]([CH2:9][CH2:10][NH:11][C:12](=[O:14])[CH3:13])=[CH:7][C:6]2[O:15][CH2:16][O:17][C:5]=2[CH:4]=1.[C-:18]#[N:19].[Na+].O>CS(C)=O>[C:18]([CH2:2][C:3]1[C:8]([CH2:9][CH2:10][NH:11][C:12](=[O:14])[CH3:13])=[CH:7][C:6]2[O:15][CH2:16][O:17][C:5]=2[CH:4]=1)#[N:19]

참가 물질

5

반응물 3

HCID 962WaterHCID 8929Sodium CyanideHCID 21824570N-(6-Chloromethyl-3,4-methylenedioxyphenethyl) acetamide

생성물 1

HCID 1236400N-{2-[6-(cyanomethyl)-1,3-benzodioxol-5-yl]ethyl}acetamide

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

4.7 g of N-(6-chloromethyl-3,4-methylenedioxyphenethyl) acetamide was dissolved in 10 ml of DMSO and 1.32 g (0.028 mole) of sodium cyanide added to the stirred solution. Within a few minutes, the temperature rose from 25° to 32° C. After 1.5 hrs at ambient temperature the mixture was poured into ice and water. The suspension was extracted with three 50-ml portions of benzene. The benzene layers were washed with saturated brine six times, then with water, the solution dried, and the solvent distilled in the rotary evaporator leaving the above-named product as a crystalline solid, m.p. 153.3-155.5.

후처리

  1. waitWithin a few minutes
  2. customrose from 25° to 32° C
  3. extractionThe suspension was extracted with three 50-ml portions of benzene
  4. washThe benzene layers were washed with saturated brine six times
  5. dry with materialwith water, the solution dried
  6. distillationthe solvent distilled in the rotary evaporator

출처 및 근거

ORD 기록
ord-8a1e2e70c97043dd951e32df7c6106a4
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04065473

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