Triethylamine → 2-Fluoro-5-((3-oxo-4,5,6,7-tetrahydroisobenzofuran-1 (3h)-ylidene)methyl)benzonitrile

HRID 925062ノート

反応式

HRID 925062 の反応式
[Br-].C([P+](CCCC)(CCCC)[CH:7]1[C:11]2[CH2:12][CH2:13][CH2:14][CH2:15][C:10]=2[C:9](=[O:16])[O:8]1)CCC.[F:25][C:26]1[CH:33]=[CH:32][C:31]([CH:34]=O)=[CH:30][C:27]=1[C:28]#[N:29].C(N(CC)CC)C>ClCCl>[F:25][C:26]1[CH:33]=[CH:32][C:31]([CH:34]=[C:7]2[C:11]3[CH2:12][CH2:13][CH2:14][CH2:15][C:10]=3[C:9](=[O:16])[O:8]2)=[CH:30][C:27]=1[C:28]#[N:29]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 27695822-Fluoro-5-formylbenzonitrileHCID 66966753Tributyl(3-oxo-1,3,4,5,6,7-hexahydro-2-benzofuran-1-yl)phosphonium bromide

生成物 1

HCID 690434422-Fluoro-5-((3-oxo-4,5,6,7-tetrahydroisobenzofuran-1 (3h)-ylidene)methyl)benzonitrile

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of EXAMPLE 1B (3.05 g) in dichloromethane (30 mL) was added 2-fluoro-5-formylbenzonitrile (1.08 g) and triethylamine (1.02 mL). The mixture was stirred at ambient temperature for 16 hours and concentrated. The concentrate was partitioned between ethyl acetate and brine. The organic layer was washed with brine and concentrated. The concentrate was purified by flash chromatography on silica gel with 50% ethyl acetate in hexane.

後処理

  1. concentrationconcentrated
  2. customThe concentrate was partitioned between ethyl acetate and brine
  3. washThe organic layer was washed with brine
  4. concentrationconcentrated
  5. customThe concentrate was purified by flash chromatography on silica gel with 50% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-080e7bc1d94a4ed0964a2514e15399a9
出典データセット
uspto-grants-2016_03
特許番号
US09283222B2

反応ノート

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