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Water → HCID 21388672、化合物

HRID 1833292
ノート
印刷プレビュー

反応式

HRID 1833292 の反応式
[NH2:1][C:2]1[C:7]([Cl:8])=[CH:6][N:5]=[C:4]([O:9][CH2:10][CH2:11][OH:12])[C:3]=1[Cl:13].[C:14](Cl)(=[O:16])[CH3:15].O>N1C=CC=CC=1>[NH2:1][C:2]1[C:7]([Cl:8])=[CH:6][N:5]=[C:4]([O:9][CH2:10][CH2:11][O:12][C:14](=[O:16])[CH3:15])[C:3]=1[Cl:13]
参加物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 6367Acetyl chlorideHCID 213886662-[(4-Amino-3,5-dichloropyridin-2-yl)oxy]ethan-1-ol

生成物 1

HCID 21388672HCID 21388672、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 22.3 grams (0.1 mole) of 4-amino-3,5-dichloro-2-(2-hydroxyethoxy)pyridine (prepared by the method of Example I) dissolved in 150 milliliters of pyridine was added dropwise, with agitation, 8.7 grams (0.11 mole) of acetylchloride. The mixture was brought to reflux (~100° C.) and held at this temperature for 1 hour. The mixture was cooled to room temperature and poured into water. The oil which separated was extracted with methylene chloride, washed with 200 milliliters of water and dried over potassium carbonate. The solvent was evaporated under reduced pressure and the 4-amino-3,5-dichloro-2-(2-acetoxyethoxy)pyridine product was recovered by recrystallization from hexane. The product was recovered in a yield of 13.7 grams which melts at 76°-77° C.

後処理

  1. temperatureto reflux (~100° C.)
  2. customThe oil which separated
  3. extractionwas extracted with methylene chloride
  4. washwashed with 200 milliliters of water
  5. dry with materialdried over potassium carbonate
  6. customThe solvent was evaporated under reduced pressure
  7. customthe 4-amino-3,5-dichloro-2-(2-acetoxyethoxy)pyridine product was recovered by recrystallization from hexane
  8. customThe product was recovered in a yield of 13.7 grams which melts at 76°-77° C.

出典と根拠

ORDレコード
ord-e286ef2f13094fe8abb3a3b2fa26f6eb
出典データセット
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04066438

反応ノート

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