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Triethylamine → ethyl N-(4-p-nitrophenyl-2-thiazolyl)carbamate

HRID 1980824
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HRID 1980824 반응식
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[CH:9][CH:8]=2)[N:6]=1.C(N(CC)CC)C.Cl[C:24]([O:26][CH2:27][CH3:28])=[O:25]>O1CCCC1>[N+:13]([C:10]1[CH:9]=[CH:8][C:7]([C:5]2[N:6]=[C:2]([NH:1][C:24](=[O:25])[O:26][CH2:27][CH3:28])[S:3][CH:4]=2)=[CH:12][CH:11]=1)([O-:15])=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 164202-Amino-4-(p-nitrophenyl)thiazole

생성물 1

HCID 5108134ethyl N-(4-p-nitrophenyl-2-thiazolyl)carbamate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In 300 ml of tetrahydrofuran, was suspended 4.42 g of 2-amino-4-p-nitrophenylthiazole, followed by a further addition of 20 ml of triethylamine. The mixture was cooled to about 5° C., to which 10.5 ml of ethyl chloroformate was added dropwise. Then, the reaction mixture was stirred at room temperature for 3.5 days. Any insoluble matter was filtered off from the reaction mixture, and the filtrate was concentrated and then washed in ethyl acetate successively with water, dilute hydrochloric acid, and water. Then, the ethyl acetate solution was concentrated to about 50 ml and the resulting crystals were separated by filtration and then subjected to column chromatography on silica gel. The reaction product was eluted with a benzene/ethyl acetate mixed solvent. The resultant product was recrystallized from ethyl acetate to obtain 2.8 g of ethyl N-(4-p-nitrophenyl-2-thiazolyl)carbamate.

후처리

  1. additionwas added dropwise
  2. filtrationAny insoluble matter was filtered off from the reaction mixture
  3. concentrationthe filtrate was concentrated
  4. washwashed in ethyl acetate successively with water, dilute hydrochloric acid, and water
  5. concentrationThen, the ethyl acetate solution was concentrated to about 50 ml
  6. customthe resulting crystals were separated by filtration
  7. washThe reaction product was eluted with a benzene/ethyl acetate mixed solvent
  8. customThe resultant product was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-996f90971ad7454daceed7c35a8d519d
출처 데이터셋
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04511574

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