Triethylamine → N-Methyl-N-(2,2-dimethoxyethyl)-2,6-dinitro-4-trifluoromethylaniline

HRID 434465

반응식

HRID 434465 반응식
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([C:11]([F:14])([F:13])[F:12])=[CH:4][C:3]=1[N+:15]([O-:17])=[O:16].[CH3:18][NH:19][CH2:20][CH:21]([O:24][CH3:25])[O:22][CH3:23].C(N(CC)CC)C>C1C=CC=CC=1>[CH3:18][N:19]([CH2:20][CH:21]([O:24][CH3:25])[O:22][CH3:23])[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([C:11]([F:14])([F:13])[F:12])=[CH:4][C:3]=1[N+:15]([O-:17])=[O:16]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 85032,2-DimethoxyethylmethylamineHCID 98094-Chloro-3,5-dinitrobenzotrifluoride

생성물 1

HCID 20492553N-Methyl-N-(2,2-dimethoxyethyl)-2,6-dinitro-4-trifluoromethylaniline

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

4-Chloro-3,5-dinitrobenzotrifluoride (5.4 grams; 0.02 mole) dissolved in benzene was charged into a glass reaction vessel equipped with a mechanical stirrer and addition funnel. N-Methyl-N-2,2-dimethoxyethylamine (2,4 grams; 0.02 mole) and triethylamine (2.02 grams; 0.02 mole) both dissolved in benzene (50 ml) were then added dropwise with stirring. After the addition was completed stirring was continued for a period of 1 hour resulting in the formation of a precipitate. The reaction mixture was filtered to remove the acid acceptor salt and was chromatographed. The solution was then evaporated to yield a solid product. This solid was recrystallized from hexane to yield the desired product N-methyl-N-(2,2-dimethoxyethyl)-2,6-dinitro-4-trifluoroemethylaniline melting at 48° to 50° C.

후처리

  1. additionwas charged into a glass reaction vessel
  2. customequipped with a mechanical stirrer and addition funnel
  3. additionwere then added dropwise
  4. additionAfter the addition
  5. stirringwas completed stirring
  6. customresulting in the formation of a precipitate
  7. filtrationThe reaction mixture was filtered
  8. customto remove the acid acceptor salt
  9. customwas chromatographed
  10. customThe solution was then evaporated
  11. customto yield a solid product
  12. customThis solid was recrystallized from hexane

출처 및 근거

ORD 기록
ord-c42d1d4d697547de80e21add2200b073
출처 데이터셋
uspto-grants-1983_08
특허 번호
US04397677

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