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Ammonia → HCID 77230828、化合物

HRID 921038
ノート
印刷プレビュー

反応式

HRID 921038 の反応式
P(Cl)(Cl)([Cl:3])=O.[C:6]([C:10]1[CH:11]=[CH:12][CH:13]=[C:14]2[C:19]=1[N:18]=[CH:17][NH:16][C:15]2=O)([CH3:9])([CH3:8])[CH3:7].N>C1(C)C=CC=CC=1.CN(C)C1C=CC=CC=1>[Cl:3][C:15]1[C:14]2[C:19](=[C:10]([C:6]([CH3:9])([CH3:8])[CH3:7])[CH:11]=[CH:12][CH:13]=2)[N:18]=[CH:17][N:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 222AmmoniaHCID 24813Phosphorus oxychlorideHCID 136278287HCID 136278287、化合物

生成物 1

HCID 77230828HCID 77230828、化合物

試薬・触媒・溶媒 2

HCID 949N,N-Dimethylaniline触媒HCID 1140Toluene溶媒2 回

実験手順

18.6 ml (200 mmol) of phosphoryl chloride are added dropwise at room temperature to a suspension of 10.2 g (50 mmol) of 8-tert-butyl-4(3H)-quinazolinone in 100 ml of toluene. After addition of 5 drops of N,N-dimethylaniline, the reaction mixture is heated under reflux for 5 h. After cooling, the reaction mixture is diluted with 300 ml of toluene, poured onto 1000 g of ice and rendered alkaline (pH about 9) by addition of conc. ammonia solution. The organic phase is separated off, washed once with 300 ml of sat. sodium chloride solution, dried over magnesium sulfat e, and the toluene is removed in vacuo. The residue is chromatographed on silica gel (n-heptane:ethyl acetate 3:1 v:v). Yield: 9.3 g (42 mmol), 84%. Purity: >95% according to 1H-NMR.

後処理

  1. temperaturethe reaction mixture is heated
  2. temperatureunder reflux for 5 h
  3. temperatureAfter cooling
  4. customThe organic phase is separated off
  5. washwashed once with 300 ml of sat. sodium chloride solution
  6. dry with materialdried over magnesium sulfat e
  7. customthe toluene is removed in vacuo
  8. customThe residue is chromatographed on silica gel (n-heptane:ethyl acetate 3:1 v:v)

出典と根拠

ORDレコード
ord-f31949a0913843b58d7b5ba35f99528f
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09273080B2

反応ノート

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