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Hydrochloric Acid → HCID 178493668, 화합물

HRID 37135
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HRID 37135 반응식
[H-].[Na+].[CH:3]([O:5][CH2:6][CH3:7])=O.[CH3:8][O:9]CC(OCC)=O.[NH2:16][C:17]1[C:21]([C:22]2[CH:27]=[CH:26][C:25]([S:28][C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[CH:24][CH:23]=2)=[CH:20][NH:19][N:18]=1.Cl>C(OCC)(=O)C.O.O1CCCC1>[OH:9][C:8]1[N:18]2[N:19]=[CH:20][C:21]([C:22]3[CH:23]=[CH:24][C:25]([S:28][C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)=[CH:26][CH:27]=3)=[C:17]2[N:16]=[CH:7][C:6]=1[O:5][CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 8025Ethyl formateHCID 24758Sodium hydrideHCID 77544Ethyl 2-methoxyacetateHCID 178509258HCID 178509258, 화합물

생성물 1

HCID 178493668HCID 178493668, 화합물

시약·촉매·용매 3

HCID 962
Water
용매
2회
HCID 8028Tetrahydrofuran용매
HCID 8857Ethyl Acetate용매

실험 절차

To a tetrahydrofuran suspension of 480 mg of 60% sodium hydride, 2 ml of ethyl formate and 1.0 g of ethyl methoxyacetate were added under nitrogen atmosphere, and the mixture was stirred for 16 hours at room temperature. In succession, adding 1.0 g of 3-amino-4(4-phenylthiophenyl)pyrazole, the solution was stirred for 4 hours in reflux. After allowing to cool, water was added and the solution was neutralized with 10% hydrochloric acid. Removing water, ethyl acetate was added, and insoluble matter was filtered. The filtrate was washed in ethyl acetate and ether and dried, and the title compound was obtained (100 mg, 8%).

후처리

  1. additionwere added under nitrogen atmosphere
  2. stirringthe solution was stirred for 4 hours
  3. temperaturein reflux
  4. temperatureto cool
  5. filtrationinsoluble matter was filtered
  6. washThe filtrate was washed in ethyl acetate
  7. dry with materialether and dried

출처 및 근거

ORD 기록
ord-907f2ec5246641ac9182ba93481bc4bb
출처 데이터셋
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05420128

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