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HCID 13271775, 화합물 → HCID 135759062, 화합물

HRID 2295976
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HRID 2295976 반응식
[Cl:1][C:2]1[CH:23]=[CH:22][C:5]2[CH:6]3[C:20](=[O:21])[NH:19][CH:18]=[N:17][CH:7]3[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:4]=2[CH:3]=1>O1CCCC1.[O-2].[O-2].[Mn+4]>[Cl:1][C:2]1[CH:23]=[CH:22][C:5]2[C:6]3[C:20](=[O:21])[NH:19][CH:18]=[N:17][C:7]=3[CH2:8][N:9]=[C:10]([C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:4]=2[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 13271775HCID 13271775, 화합물

생성물 1

HCID 135759062HCID 135759062, 화합물

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 2.2 g (6.8 mmol) of 9-chloro-4a,11b-dihydro-7-phenyl-5H-pyrimido[4,5-d][2]benzazepin-1(2H)-one and 10 g (110 mmol) of activated manganese dioxide in 100 mL of tetrahydrofuran was refluxed for 18 hr. The mixture was cooled, the manganese dioxide was removed by filtration over celite and the filtrate was concentrated at reduced pressure. Purification of the residue by column chromatography (silica gel 10 g; eluents, 20% ether in methylene chloride followed by 50% ethyl acetate in methylene chloride) gave pale yellow prisms, mp 226°-229°.

후처리

  1. temperaturewas refluxed for 18 hr
  2. temperatureThe mixture was cooled
  3. customthe manganese dioxide was removed by filtration over celite
  4. concentrationthe filtrate was concentrated at reduced pressure
  5. customPurification of the residue by column chromatography (silica gel 10 g; eluents, 20% ether in methylene chloride followed by 50% ethyl acetate in methylene chloride)
  6. customgave pale yellow prisms, mp 226°-229°

출처 및 근거

ORD 기록
ord-c5cd879811e846538023ce8103428ff2
출처 데이터셋
uspto-grants-1984_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04427589

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