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Triethylamine → HCID 53744793、化合物

HRID 1060579
ノート
印刷プレビュー

反応式

HRID 1060579 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 8471TriethylamineHCID 133894-Pyridinecarboxaldehyde

生成物 1

HCID 53744793HCID 53744793、化合物収率 60.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-16baf9cafe6247c49cbb9f37b588ef49
出典データセット
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06525055B1

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート