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Hydrochloric Acid → HCID 19962752, 화합물

HRID 52013
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HRID 52013 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([O:11][C:12]2[CH:20]=[CH:19][C:18]3[NH:17][C:16]([CH3:21])=[C:15]([N+:22]([O-])=O)[C:14]=3[C:13]=2[C:25]([O:27][CH2:28][CH:29]=[CH2:30])=[O:26])[N:4]=1.Cl.[Sn]>CO>[NH2:22][C:15]1[C:14]2[C:13]([C:25]([O:27][CH2:28][CH:29]=[CH2:30])=[O:26])=[C:12]([O:11][C:5]3[N:6]=[C:7]([O:9][CH3:10])[CH:8]=[C:3]([O:2][CH3:1])[N:4]=3)[CH:20]=[CH:19][C:18]=2[NH:17][C:16]=1[CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 5352426Tin atomHCID 19962765HCID 19962765, 화합물

생성물 1

HCID 19962752HCID 19962752, 화합물수율 79.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

3.4 g of allyl 5-[(4,6-dimethoxypyrimidin-2-yl)oxy]-2-methyl-3-nitroindol-4-carboxylate was dissolved in 50 ml of methanol, and 5 ml of concentrated hydrochloric acid was added thereto. Then, 4.9 g of tin powder was gradually added at room temperature. Them, the mixture was stirred at room temperature for 12 hours. The solid was filtered off, and then residue was concentrated under reduced pressure and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous sodium sulfate. The residue obtained by concentration under reduced pressure, was crystallized from isopropyl ether to obtain 2.5 g (yield: 79%) of the desired product. mp: 132°-135° C.

후처리

  1. filtrationThe solid was filtered off
  2. concentrationresidue was concentrated under reduced pressure
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe residue obtained by concentration under reduced pressure
  7. customwas crystallized from isopropyl ether

출처 및 근거

ORD 기록
ord-172b663c480f428491802387607eff65
출처 데이터셋
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05616537

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