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Phenacyl bromide → HCID 23463072, 화합물

HRID 2286338
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HRID 2286338 반응식
[NH2:1][C:2]1[S:3][C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[Cl:13])=[N:5][N:6]=1.NNC(N)=S.ClC1C=CC=CC=1C(Cl)=O.Br[CH2:30][C:31]([C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)=O>CN(C)C=O>[Cl:13][C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=1[C:4]1[S:3][C:2]2=[N:1][C:31]([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)=[CH:30][N:6]2[N:5]=1
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참가 물질

6

반응물 4

HCID 6259Phenacyl bromideHCID 691102-Chlorobenzoyl chlorideHCID 5542115-(2-Chlorophenyl)-1,3,4-thiadiazol-2-amineHCID 2723789Thiosemicarbazide

생성물 1

HCID 23463072HCID 23463072, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

10.5 g (0.05 mol) of 2-amino-5-(2-chlorophenyl)-1,3,4-thiadiazole, melting point 189,5° C. (prepared by reacting thiosemicarbazide with 2-chlorobenzoyl chloride) together with 10 g (0.05 mol) of bromoacetophenone are warmed to 120° C. in 100 ml of dimethylformamide for 3 hours and the mixture is then cooled and concentrated in a rotary evaporator. After digesting the residue with water, the digestion mixture is filtered and the residue is recrystallised from alcohol. A second fraction is obtained by concentrating the alcoholic mother liquor. A total yield of 12.5 g, corresponding to 80% of theory, of colourless crystals of melting point 126° C. is obtained.

후처리

  1. temperaturethe mixture is then cooled
  2. concentrationconcentrated in a rotary evaporator
  3. filtrationthe digestion mixture is filtered
  4. customthe residue is recrystallised from alcohol
  5. customA second fraction is obtained
  6. concentrationby concentrating the alcoholic mother liquor
  7. customA total yield of 12.5 g, corresponding to 80% of theory, of colourless crystals of melting point 126° C. is obtained

출처 및 근거

ORD 기록
ord-9f593c31b76e42e983b3e5a8b3cec8a0
출처 데이터셋
uspto-grants-1981_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04265898

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