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Triethylamine → HCID 53744793、化合物

HRID 2300048
ノート
印刷プレビュー

反応式

HRID 2300048 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

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 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.

後処理

  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

出典と根拠

ORDレコード
ord-23225ce39f8d4dcd9c62056a477b5cc0
出典データセット
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06498160B2

反応ノート

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