Methyl iodide → HCID 13280935、化合物

HRID 1903630ノート

反応式

HRID 1903630 の反応式
[Cl:1][C:2]1[CH:23]=[CH:22][C:5]2[C:6]3[C:7](=[CH:18][NH:19][C:20]=3[CH3:21])[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1.[CH3:24]C(C)([O-])C.[K+].CI>CN(C)C=O.O>[Cl:1][C:2]1[CH:23]=[CH:22][C:5]2[C:6]3[C:7](=[CH:18][N:19]([CH3:24])[C:20]=3[CH3:21])[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 13067111HCID 13067111、化合物HCID 23665647Potassium tert-butoxide

生成物 1

HCID 13280935HCID 13280935、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

In one portion, 2.0 g (5.8) mmol) of 8-chloro-6-(2-chlorophenyl)-1-methyl-2H,4H-pyrrolo[3,4-d][2]benzazepine were added to an ice-cooled solution of 0.8 g (7.1 mmol) of potassium t-butoxide in 20 ml of dry dimethylformamide. After stirring at 0° C. for 10 minutes, 0.8 ml (12.8 mmol) of methyl iodide was added and the resulting solution was stirred for 20 minutes. The mixture was diluted with water, and the resulting precipitate was collected by filtration. The solid was dissolved in methylene chloride, dried over anhydrous sodium sulfate, and concentrated at reduced pressure to give 8-chloro-6-(2-chlorophenyl)-1,2-dimethyl-2H,4H-pyrrolo[3,4-d][2]benzazepine as orange prisms, mp 200°-202° C. A sample was recrystallized from a mixture of ether and methylene chloride to give pale yellow prisms, mp 203°-204° C.

後処理

  1. stirringthe resulting solution was stirred for 20 minutes
  2. filtrationthe resulting precipitate was collected by filtration
  3. dissolutionThe solid was dissolved in methylene chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated at reduced pressure

出典と根拠

ORDレコード
ord-29830dc37f8c4bac96ca648e2188f01b
出典データセット
uspto-grants-1984_03
特許番号
US04436662

反応ノート

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