Sodium Hydroxide → HCID 135752、化合物

HRID 1156551ノート

反応式

HRID 1156551 の反応式
[I-].[CH3:2][O:3][C:4]1[CH:5]=[C:6]([C:10]23[CH2:18][CH2:17][CH2:16][CH2:15][CH:14]2[N+:13]([CH3:20])([CH3:19])[CH2:12][CH2:11]3)[CH:7]=[CH:8][CH:9]=1.[OH-].[Na+]>O>[CH3:2][O:3][C:4]1[CH:5]=[C:6]([C:10]2([CH2:11][CH2:12][N:13]([CH3:20])[CH3:19])[CH2:18][CH2:17][CH2:16][CH:15]=[CH:14]2)[CH:7]=[CH:8][CH:9]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 12838431Hexahydro-3a-(m-methoxyphenyl)-1,1-dimethyl-indolinium iodide

生成物 1

HCID 135752HCID 135752、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
170 °C

実験手順

1 g of hexahydro-3a-(m-methoxyphenyl)-1,1-dimethyl-indolinium iodide is dissolved in 40 ml of water. The solution is applied to a column containing 50 g of Amberlite IRA 400 (pre-treated with sodium hydroxide; washed with distilled water until neutral). Thereafter, the column is eluted with 500 ml of distilled water. After distillation of the water, the hexahydro-3a-(m-methoxyphenyl)-1,1-dimethyl-indolinium hydroxide remaining as the residue is heated at 170° C. in a distillation apparatus in a high vacuum, an oil distilling over. This oil still contains, besides rac. 1-(m-methoxyphenyl)-N,N-dimethyl-2-cyclohexene-1-ethylamine, a relatively small amount of hexahydro-3a-(m-methoxyphenyl)-1-methylindoline.

後処理

  1. additioncontaining
  2. washThereafter, the column is eluted with 500 ml of distilled water
  3. distillationAfter distillation of the water
  4. distillationan oil distilling over

出典と根拠

ORDレコード
ord-3451f4011ef54887bec9423424974797
出典データセット
uspto-grants-1982_06
特許番号
US04336268

反応ノート

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