Methyl iodide → HCID 13280935, 화합물

HRID 1903630노트

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HRID 1903630 반응식
[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

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 13067111HCID 13067111, 화합물HCID 23665647Potassium tert-butoxide

생성물 1

HCID 13280935HCID 13280935, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-29830dc37f8c4bac96ca648e2188f01b
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04436662

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