Dibutyltin oxide → HCID 178466679、化合物

HRID 510843ノート

反応式

HRID 510843 の反応式
[C:1]([C:4]1[CH:5]=[C:6]([Cl:20])[C:7]([CH3:19])=[C:8]([C:17]#[N:18])[C:9]=1[C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[CH:11]=1)(=[O:3])[CH3:2].[N:21]([Si](C)(C)C)=[N+:22]=[N-:23].C([Sn](CCCC)=O)CCC>C1(C)C=CC=CC=1>[Cl:20][C:6]1[C:7]([CH3:19])=[C:8]([C:17]2[NH:23][N:22]=[N:21][N:18]=2)[C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[CH:11]=2)=[C:4]([C:1](=[O:3])[CH3:2])[CH:5]=1

参加物

5

反応物 3

HCID 61221Dibutyltin oxideHCID 78378AzidotrimethylsilaneHCID 583684696-Acetyl-4-chloro-3'-fluoro-3-methylbiphenyl-2-carbonitrile

生成物 1

HCID 178466679HCID 178466679、化合物収率 85.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 6-acetyl-4-chloro-3′-fluoro-3-methylbiphenyl-2-carbonitrile (100 mg, 0.3 mmol), azidotrimethylsilane (0.092 mL, 0.69 mmol), and dibutyloxostannane (13 mg, 0.052 mmol) in toluene (2.9 mL) was heated at reflux overnight. The mixture was evaporated to dryness and purified on silica gel, eluting with 0 to 50% ethyl acetate in hexane, to give the desired product (85 mg, 70%). LCMS calculated for C16H13ClFN4O (M+H)+: m/z=331.1. found: 331.0.

後処理

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. customThe mixture was evaporated to dryness
  4. custompurified on silica gel
  5. washeluting with 0 to 50% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-ec571eb1cb6548bab1984680df6919c1
出典データセット
uspto-grants-2015_08
特許番号
US09096600B2

反応ノート

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