ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Toluene → HCID 54212925、化合物

HRID 619118
ノート
印刷プレビュー

反応式

HRID 619118 の反応式
C[Si]([C:5]#[N:6])(C)C.I[C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[N:14]([CH3:18])[C:13](=[O:19])[CH:12]=[C:11]2[CH2:20][C:21]([O:23][CH3:24])=[O:22].CNC1C=CC(I)=CC=1.C1(C)C=CC=CC=1>C(N(CC)CC)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O>[C:5]([C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[N:14]([CH3:18])[C:13](=[O:19])[CH:12]=[C:11]2[CH2:20][C:21]([O:23][CH3:24])=[O:22])#[N:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 1140TolueneHCID 82115Trimethylsilyl cyanideHCID 6454006Benzenamine, 4-iodo-N-methyl-HCID 54160516HCID 54160516、化合物

生成物 1

HCID 54212925HCID 54212925、化合物

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒
HCID 962Water溶媒
HCID 8471Triethylamine溶媒

実験手順

1.1 ml of trimethylsilyl cyanide (8.4 mmol) followed by 0.15 g (0.13 mmol) of tetrakistriphenylphosphinepalladium are added to a solution of 0.50 g (1.4 mmol) of methyl 6-iodo-1-methyl-2-oxo-1,2-dihydro-4-quinolineacetate (prepared from N-methyl-4-iodoaniline according to the method described in Example 1) in 6 ml of anhydrous triethylamine. The reaction medium is then heated to reflux for 4 hours under a nitrogen atmosphere. After cooling to room temperature, the medium is poured into 60 ml of toluene and 60 ml of water. The organic phase is washed with water and the initial aqueous phase is re-extracted with dichloromethane. The organic phases are combined, dried over sodium sulphate and concentrated under vacuum. The residue is purified by flash chromatography on silica, eluting with a methanol/dichloromethane (5:95) mixture.

後処理

  1. temperatureThe reaction medium is then heated
  2. temperatureto reflux for 4 hours under a nitrogen atmosphere
  3. washThe organic phase is washed with water
  4. extractionthe initial aqueous phase is re-extracted with dichloromethane
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated under vacuum
  7. customThe residue is purified by flash chromatography on silica
  8. washeluting with a methanol/dichloromethane (5:95) mixture

出典と根拠

ORDレコード
ord-f7d3515961e94f28b1cf521790e78106
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05958924

反応ノート

読み込み中…

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