4-Chloro-3-nitrobenzophenone → {4-[Methyl(octyl)amino]-3-nitrophenyl}(phenyl)methanone

HRID 27379

반응식

HRID 27379 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:15]=[CH:16][C:17]=1Cl)[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:8])([O-:3])=[O:2].[CH3:19][NH:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]>C(O)C>[N+:1]([C:4]1[CH:5]=[C:6]([CH:15]=[CH:16][C:17]=1[N:20]([CH3:19])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:8])([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 417434-Chloro-3-nitrobenzophenoneHCID 75538Octylmethylamine

생성물 1

HCID 23342777{4-[Methyl(octyl)amino]-3-nitrophenyl}(phenyl)methanone

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 9.23 g. of 3-nitro-4-chloro-benzophenone, 10 ml. of ethanol and 10.3 g. of N-methyl-N-octylamine is stirred at 80° to 85° C. for 30 minutes, and then the mixture is poured onto 100 ml. of ice water. The aqueous phase is extracted with 2×75 ml. of benzene. The benzene phases are combined, washed with distilled water until chloride-free, dried over anhydrous magnesium sulphate, filtered, and evaporated in vacuo. 11.57 g. of 3-nitro-4-(N-methyl-N-octylamino)-benzophenone are obtained in the form of an oily residue. On the basis of thin layer chromatographical examination, a pure, uniform product is obtained.

후처리

  1. additionA mixture of 9.23 g
  2. additionthe mixture is poured onto 100 ml
  3. extractionThe aqueous phase is extracted with 2×75 ml
  4. washwashed with distilled water until chloride-free
  5. dry with materialdried over anhydrous magnesium sulphate
  6. filtrationfiltered
  7. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-f293bf93d94348b09e6e14922f208abc
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04221739

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