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Diethyl Ether → HCID 135705321, 화합물

HRID 1283170
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HRID 1283170 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13]CC1C=CC=CC=1)[N:9]=[C:8]1[N:21]=[C:22]([C:26]([O:28][CH2:29][CH3:30])=[O:27])[NH:23][C:24](=[O:25])[C:7]1=[CH:6]2.CCOCC>FC(F)(F)C(O)=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[OH:13])[N:9]=[C:8]1[N:21]=[C:22]([C:26]([O:28][CH2:29][CH3:30])=[O:27])[NH:23][C:24](=[O:25])[C:7]1=[CH:6]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3283Diethyl EtherHCID 135705342HCID 135705342, 화합물

생성물 1

HCID 135705321HCID 135705321, 화합물수율 6%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of ethyl 7-methoxy-8-benzyloxypyrimido[4,5-b]quinolin-4(3H)one-2-carboxylate (198 mg., 0.488 mmole) in trifluoroacetic acid (4 ml.) is stirred at room temperature for 8 days. Ether (15 ml.) is added and the yellow precipitate which forms separated by filtration. It is taken up in chloroform and the solution filtered through diatomaceous earth to remove a small amount of insoluble material. The filtrate is decolorized with charcoal and concentrated under reduced pressure to small volume. The solid which forms is filtered and dried; 9 mg., 6% yield; m.p. 265°-266°C. (dec.).

후처리

  1. customthe yellow precipitate which forms separated by filtration
  2. filtrationthe solution filtered through diatomaceous earth
  3. customto remove a small amount of insoluble material
  4. concentrationconcentrated under reduced pressure to small volume
  5. filtrationThe solid which forms is filtered
  6. customdried

출처 및 근거

ORD 기록
ord-2059bc824cb34f8eb5ece5f919624eee
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03974161

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