Triethylamine → 2-(Chloromethyl)-1-(2,6-dichlorobenzyl)-4-nitro-1H-imidazole

HRID 714633노트

반응식

HRID 714633 반응식
[Cl:1][C:2]1[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[C:3]=1[CH2:4][N:5]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[N:7]=[C:6]1[CH2:13]O.C(N(CC)CC)C.S(Cl)([Cl:29])=O>ClCCl>[Cl:29][CH2:13][C:6]1[N:5]([CH2:4][C:3]2[C:2]([Cl:1])=[CH:18][CH:17]=[CH:16][C:15]=2[Cl:19])[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[N:7]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 24386Thionyl Chloride2회HCID 67410386[1-(2,6-Dichlorobenzyl)-4-nitro-1H-imidazol-2-yl]methanol

생성물 1

HCID 674099292-(Chloromethyl)-1-(2,6-dichlorobenzyl)-4-nitro-1H-imidazole

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

210 mg (0.70 mmol) of the compound from Example 37A were dissolved in 10 ml of dichloromethane, and 145 μl (1.04 mmol) of triethylamine and 61 μl (0.83 mmol) of thionyl chloride were added at 0° C. The mixture was stirred at RT for 24 h. A further 200 μl (2.72 mmol) of thionyl chloride were then added, and the mixture was stirred under reflux for 15 min. Under reduced pressure, the reaction mixture was then freed from all volatile components. This gave, in a purity of 88%, 200 mg (80% of theory) of the target compound, which was reacted further without any further purification.

후처리

  1. stirringthe mixture was stirred
  2. temperatureunder reflux for 15 min
  3. customThis gave, in a purity of 88%, 200 mg (80% of theory) of the target compound, which was reacted further without any further purification

출처 및 근거

ORD 기록
ord-7ca9cbf52d864006b20986c798521ac7
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187466B2

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