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

HRID 462098ノート

反応式

HRID 462098 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8a1e2e70c97043dd951e32df7c6106a4
出典データセット
uspto-grants-1977_12
特許番号
US04065473

反応ノート

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