1,2-Dichloroethane → N-dimethylaminomethyleneguanine

HRID 274998노트

반응식

HRID 274998 반응식
[CH3:1][N:2]([CH3:5])[CH:3]=O.S(Cl)(Cl)=O.ClCCCl.[NH:14]1[C:23](=[O:24])[C:22]2[NH:21][CH:20]=[N:19][C:18]=2[N:17]=[C:15]1[NH2:16]>O>[CH3:1][N:2]([CH:5]=[N:16][C:15]1[NH:14][C:23](=[O:24])[C:22]2[NH:21][CH:20]=[N:19][C:18]=2[N:17]=1)[CH3:3]

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 135398634Guanine

생성물 1

HCID 136087653N-dimethylaminomethyleneguanine수율 85%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

131.6 g (1.8 mol) of N,N-dimethylformamide and 42.8 g (0.36 mol) of thionyl chloride were added to 500 ml of 1,2-dichloroethane, and then 45.3 g (0.3 mol) of guanine (manufactured by Sumika Fine Chemicals Co., Ltd.) was added, followed by stirring at 80° C. for 6 hours. After cooling, the reaction mixture was added to 1000 ml of water to separate out the water layer, and then the water layer was neutralized with sodium hydrogen carbonate. The precipitating crystal was collected by filtration and washed with 100 ml of water to yield 52.6 g (0.255 mol) of a white crystal of N-dimethylaminomethyleneguanine (yield 85%).

후처리

  1. temperatureAfter cooling
  2. customto separate out the water layer
  3. filtrationThe precipitating crystal was collected by filtration
  4. washwashed with 100 ml of water

출처 및 근거

ORD 기록
ord-cbd837ab981b433dbf02f01d16d5a464
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05391733

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