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Triethylamine → HCID 53744793, 화합물

HRID 1060579
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HRID 1060579 반응식
C(N(CC)CC)C.[CH3:8][O:9][C:10]1[CH:11]=[C:12]2[C:16](=[CH:17][C:18]=1[O:19][CH3:20])[C:15](=[O:21])[O:14][CH:13]2[PH2](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[N:41]1[CH:46]=[CH:45][C:44]([CH:47]=O)=[CH:43][CH:42]=1>C(Cl)Cl>[CH3:8][O:9][C:10]1[CH:11]=[C:12]2[C:16](=[CH:17][C:18]=1[O:19][CH3:20])[C:15](=[O:21])[O:14][C:13]2=[CH:47][C:44]1[CH:45]=[CH:46][N:41]=[CH:42][CH:43]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8471TriethylamineHCID 133894-Pyridinecarboxaldehyde

생성물 1

HCID 53744793HCID 53744793, 화합물수율 60.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Triethylamine (20 ml, 145 mmoles) was dropwise added to a suspension of 5,6-dimethoxy-3-(triphenyl-λ6-phosphanyl)-3H-isobenzofuran-1-one (78 g, 145 mmoles), obtained as described in example 3, and 4-pyridincarboxaldehyde (13 ml, 145 mmoles) in CH2Cl2 (1 l), at room temperature under stirring. After 1.5 hours the mixture was filtered and evaporated and the residue was treated with ethanol under reflux, cooled and filtered. The mother liquors were chromatographed (eluent: 100% CH2Cl2, then with 1% CH3OH) and the residue was brought to dryness and joined to the above filtrate to give 25 g of the title compound.

후처리

  1. customobtained
  2. filtrationAfter 1.5 hours the mixture was filtered
  3. customevaporated
  4. additionthe residue was treated with ethanol
  5. temperatureunder reflux
  6. temperaturecooled
  7. filtrationfiltered
  8. customThe mother liquors were chromatographed (eluent

출처 및 근거

ORD 기록
ord-16baf9cafe6247c49cbb9f37b588ef49
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06525055B1

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