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Triethylamine → HCID 53744793, 화합물

HRID 1250855
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HRID 1250855 반응식
C(N(CC)CC)C.[Br-].[CH3:9][O:10][C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][C:19]=1[O:20][CH3:21])[CH:16]([P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[O:15][C:14]2=[O:41].[N:42]1[CH:47]=[CH:46][C:45]([CH:48]=O)=[CH:44][CH:43]=1>C(Cl)Cl>[CH3:21][O:20][C:19]1[CH:18]=[C:17]2[C:13](=[CH:12][C:11]=1[O:10][CH3:9])[C:14](=[O:41])[O:15][C:16]2=[CH:48][C:45]1[CH:46]=[CH:47][N:42]=[CH:43][CH:44]=1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 133894-PyridinecarboxaldehydeHCID 11466779(5,6-Dimethoxy-3-oxo-1,3-dihydro-isobenzofuran-1-yl)-triphenylphosphonium bromide

생성물 1

HCID 53744793HCID 53744793, 화합물수율 60.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Triethylamine (20 ml, 145 mmoles) was added dropwise to a suspension of (5,6-dimethoxy-3-oxo-1,3-dihydro-isobenzofuran-1-yl)-triphenylphosphonium bromide (78 g, 145 mmoles), obtained as described in example 12, and 4-pyridincarboxaldehyde (13.0 ml, 145 mmoles) in methylene chloride (1 l), at room temperature, under stirring. After 1.5 hours the mixture was filtered and evaporated and the residue was treated with boiling ethanol, cooled and filtered. The mother liquors were chromatographed (eluent: methylene chloride then with 1% methanol) 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 boiling ethanol
  5. temperaturecooled
  6. filtrationfiltered
  7. customThe mother liquors were chromatographed (eluent

출처 및 근거

ORD 기록
ord-8abde112937e4afcb0f61cefbfce3e67
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06340684B1

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