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Hydrochloric Acid → 4-[1-(4-Methoxyphenyl)ethenyl]-N,N-dimethylaniline

HRID 1763168
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HRID 1763168 반응식
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([C:7]([C:9]2[CH:14]=[CH:13][C:12]([N:15]([CH3:17])[CH3:16])=[CH:11][CH:10]=2)=O)=[CH:5][CH:4]=1.O1CCC[CH2:21]1.O.Cl>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([C:7]([C:9]2[CH:14]=[CH:13][C:12]([N:15]([CH3:17])[CH3:16])=[CH:11][CH:10]=2)=[CH2:21])=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 8028TetrahydrofuranHCID 2825054(4-(Dimethylamino)phenyl)(4-methoxyphenyl)methanone

생성물 1

HCID 156067734-[1-(4-Methoxyphenyl)ethenyl]-N,N-dimethylaniline

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Separately, a solution was prepared by mixing 18.2 g of 4-methoxy-4'-dimethylaminobenzophenone (melting at 126°-127° C.) and 100 ml of tetrahydrofurane, and the solution was slowly added to the liquid reaction mixture and the whole matter was stirred for one hour at a temperature of 40° to 50° C. Then the whole matter was mixed with 400 ml of water and 300 ml of toluene and after making the mixture weakly acidic by dilute hydrochloric acid, the acidified mixture was stirred for a whole at 80° C. and separated into an aqueous layer and an organic layer (toluene layer). After adding activated carbon to the toluene layer and filtering the layer while hot, toluene was distilled off from the filtrate to obtain 17.1 g of 1-(p-methoxyphenyl)-1-(p-dimethylaminophenyl)ethylene of pale yellow in color, melting at 123°-125° C.

후처리

  1. customSeparately, a solution was prepared
  2. additionthe solution was slowly added to the liquid reaction mixture
  3. stirringthe acidified mixture was stirred for a whole at 80° C.
  4. customseparated into an aqueous layer
  5. additionAfter adding activated carbon to the toluene layer
  6. filtrationfiltering the layer while hot, toluene
  7. distillationwas distilled off from the filtrate

출처 및 근거

ORD 기록
ord-93de7a3697854c91ac84405c2b59bb73
출처 데이터셋
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04835291

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