Acrylonitrile → HCID 70631280、化合物

HRID 259116ノート

反応式

HRID 259116 の反応式
[C:1](#[N:4])[CH:2]=[CH2:3].[CH3:5][O:6][CH:7]1[C:16]2[CH2:15][CH2:14][CH2:13][CH:12]3[CH2:17][CH2:18][O:19][C:10]([C:11]=23)=[CH:9][N:8]1[O:20][CH3:21].[OH-].[Na+]>O1CCOCC1>[C:1]([CH2:2][CH2:3][CH:14]1[CH2:15][C:16]2[CH:7]([O:6][CH3:5])[N:8]([O:20][CH3:21])[CH:9]=[C:10]3[O:19][CH2:18][CH2:17][CH:12]([C:11]=23)[CH2:13]1)#[N:4]

参加物

5

反応物 3

HCID 7855AcrylonitrileHCID 14798Sodium HydroxideHCID 20523931HCID 20523931、化合物

生成物 1

HCID 70631280HCID 70631280、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A solution of acrylonitrile (12 ml) and 1,2,3a,4,5,6-hexahydro-7,8-dimethoxypyrano[2,3,4-de]isoquinoline (11 g), described in Example 56, in dioxane (80 ml) and 10% NaOH solution (2.5 ml) is heated and stirred on the steam bath for 24 hr. The mixture is evaporated and the residue is dissolved in a mixture of ether and a little chloroform. The solution is extracted with 2N HCl and the extracts are washed (brine), dried and evaporated. The residue is crystallized from ether and then from benzene-hexane to give the title compound, m.p. 105°-107° C.

後処理

  1. customThe mixture is evaporated
  2. dissolutionthe residue is dissolved in a mixture of ether
  3. extractionThe solution is extracted with 2N HCl
  4. washthe extracts are washed (brine)
  5. customdried
  6. customevaporated
  7. customThe residue is crystallized from ether

出典と根拠

ORDレコード
ord-93bb737e32da4709a20e36224059ef9a
出典データセット
uspto-grants-1977_07
特許番号
US04036842

反応ノート

読み込み中…