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Chloroform → 2-bromo-N-(4-oxo-1-benzopyran-3-yl)-acetamide

HRID 2057890
ノート
印刷プレビュー

反応式

HRID 2057890 の反応式
C(Cl)(Cl)Cl.[NH2:5][C:6]1[C:15](=[O:16])[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[O:8][CH:7]=1.C(N(CC)C(C)C)(C)C.[Br:26][CH2:27][C:28](Cl)=[O:29]>C1(C)C=CC=CC=1>[Br:26][CH2:27][C:28]([NH:5][C:6]1[C:15](=[O:16])[C:14]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[O:8][CH:7]=1)=[O:29]
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

6

反応物 4

HCID 6212ChloroformHCID 81531DiisopropylethylamineHCID 89602Bromoacetyl chlorideHCID 122586463-Aminochromone

生成物 1

HCID 205422152-bromo-N-(4-oxo-1-benzopyran-3-yl)-acetamide

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
40 °C

実験手順

10 ml of chloroform are added to 8 g of 3-aminochromone in 200 ml of toluene and the mixture is warmed to 40° C. After cooling to 20° C., 10 ml of N,N-diisopropylethylamine are added with stirring, followed by the addition of 4.8 ml of bromoacetyl chloride in 20 ml of toluene at 10° C. in the course of 5 minutes. When the addition is complete, the reaction mixture is stirred for 1 hour at room temperature. The crystalline precipitate which has formed is collected by suction, washed with water and recrystallised from ethanol/petroleum ether, yielding 11.8 g of 2-bromo-N-(4-oxo-1-benzopyran-3-yl)-acetamide with a melting point of 198° C.

後処理

  1. temperatureAfter cooling to 20° C.
  2. additionWhen the addition
  3. stirringthe reaction mixture is stirred for 1 hour at room temperature
  4. customThe crystalline precipitate which has formed
  5. customis collected by suction
  6. washwashed with water
  7. customrecrystallised from ethanol/petroleum ether

出典と根拠

ORDレコード
ord-1862af8d3b1643eaa6114f456b45a01c
出典データセット
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04213980

反応ノート

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