Acetyl chloride → HCID 22668555, 화합물

HRID 1883729노트

반응식

HRID 1883729 반응식
[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][NH:5][C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][CH:7]=1.C(N(CC)CC)C.[C:23](Cl)(=[O:25])[CH3:24]>C(Cl)Cl>[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][N:5]([C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][CH:7]=1)[C:23](=[O:25])[CH3:24]

참가 물질

5

반응물 3

HCID 6367Acetyl chloride2회HCID 8471Triethylamine2회HCID 22569398HCID 22569398, 화합물

생성물 1

HCID 22668555HCID 22668555, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3.6 g of 4-(2-dimethylamino-ethylamino)-nitrobenzene (according to Gabbay et al., J. Am. Chem. Soc. 91, 5136 (1969)) are dissolved in 50 ml of methylene chloride and 5.0 ml of triethylamine are added. 1.3 ml of acetyl chloride are slowly added dropwise to this mixture at room temperature and the mixture is stirred for 2 hours at room temperature. After this time another 5.0 ml of triethylamine and 1.3 ml of acetylchloride are added and the mixture is refluxed for another 2 hours. The solvent is removed, the residue is taken up in ethyl acetate and the organic phase is extracted twice with water. After drying over MgSO4 the solvent is removed and the residue dried in vacuo.

후처리

  1. temperaturethe mixture is refluxed for another 2 hours
  2. customThe solvent is removed
  3. extractionthe organic phase is extracted twice with water
  4. dry with materialAfter drying over MgSO4 the solvent
  5. customis removed
  6. customthe residue dried in vacuo

출처 및 근거

ORD 기록
ord-43b54c6d082b4b848d95077a75a21096
출처 데이터셋
uspto-grants-2004_07
특허 번호
US06762180B1

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