Ethyl chloroformate → HCID 18615633、化合物

HRID 1271748ノート

反応式

HRID 1271748 の反応式
[Cl:1][C:2]1[C:8]([F:9])=[CH:7][C:5]([NH2:6])=[C:4]([F:10])[CH:3]=1.Cl[C:12]([O:14][CH2:15][CH3:16])=[O:13]>N1C=CC=CC=1>[Cl:1][C:2]1[C:8]([F:9])=[CH:7][C:5]([NH:6][C:12](=[O:13])[O:14][CH2:15][CH3:16])=[C:4]([F:10])[CH:3]=1

参加物

4

反応物 2

HCID 10928Ethyl chloroformateHCID 146245254-Chloro-2,5-difluoroaniline

生成物 1

HCID 18615633HCID 18615633、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

4-Chloro-2,5-difluoroaniline (XXXIX) (2.1 g, 12.8 mmol) was mixed with pyridine (20 ml) at 0° C., to it was dropwise added ethyl chloroformate (1.5 g, 13.8 mmol). After stirring for 2.5 hr while temperature slowly raised to room temperature, pyridine was evaporated and the residue crystallized in ice-water (100 ml). The crystals were filtered, washed with water and dried in fume hood overnight (2.7 g). 1H NMR (CDCl3, 300 MHz) 1.33 (3H, t, J=7.1 Hz), 4.23 (2H, q, J=7.1 Hz), 6.89 (1H, br), 7.12 (1H, dd, J=6.5, 6.5 Hz), 8.05 (1H, dd, J=7.8, 9.6 Hz) ppm.

後処理

  1. custompyridine was evaporated
  2. customthe residue crystallized in ice-water (100 ml)
  3. filtrationThe crystals were filtered
  4. washwashed with water
  5. customdried in fume hood overnight (2.7 g)

出典と根拠

ORDレコード
ord-ce5fb2f08e754adc964a18ac9ea0227c
出典データセット
uspto-grants-2007_04
特許番号
USRE039590E1

反応ノート

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