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Water → HCID 69283695、化合物

HRID 1293450
ノート
印刷プレビュー

反応式

HRID 1293450 の反応式
[CH3:1][O:2][C:3]1[C:15]2[NH:14][C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7]=2[CH:6]=[CH:5][CH:4]=1.O.CN([CH:20]=[O:21])C>O=P(Cl)(Cl)Cl>[CH:20]([N:14]1[C:15]2[C:3]([O:2][CH3:1])=[CH:4][CH:5]=[CH:6][C:7]=2[C:8]2[C:13]1=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:21]
参加物反応条件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 962WaterHCID 6228Dimethylformamide2 回HCID 107743051-methoxy-9H-carbazole

生成物 1

HCID 69283695HCID 69283695、化合物収率 96%

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

反応条件

温度
0 °C

実験手順

In a 50 mL round bottomed flask was dissolved POCl3 (0.6 mL, 15.23 mM) in 20 mL of dry DMF. The reaction mixture was stirred at 0° C. in an ice bath. To this was added slowly, 1-methoxy-9H-carbazole (1 g, 5.07 mM) dissolved in 30 mL of dry DMF. The reaction mixture was stirred for 2 hrs. Water was added to the reaction mixture and the precipitated product was filtered off. The residue was dissolved in EtOAc and was washed with brine and dried over anh. Na2SO4. Ethyl acetate was then evaporated to obtain the desired product as a white fluffy solid with a yield of 96% (1.1 g); mp 161-163° C.

後処理

  1. additionTo this was added slowly
  2. stirringThe reaction mixture was stirred for 2 hrs
  3. filtrationthe precipitated product was filtered off
  4. dissolutionThe residue was dissolved in EtOAc
  5. washwas washed with brine
  6. dry with materialdried over anh. Na2SO4
  7. customEthyl acetate was then evaporated

出典と根拠

ORDレコード
ord-7557f0b913a1412abfd3ce55d2f414b8
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07238725B2

反応ノート

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