2-Chloro-N,N-dimethylethylamine → HCID 85439121、化合物

HRID 442028ノート

反応式

HRID 442028 の反応式
[Cl:1][CH2:2][CH2:3][N:4]([CH3:6])[CH3:5].[Na].[Cl:8][C:9]1[CH:22]=[CH:21][C:12]([C:13](=[N:15][O:16][CH2:17][C:18]([OH:20])=[O:19])[CH3:14])=[CH:11][CH:10]=1>CN(C)C=O.O>[ClH:1].[CH3:5][N:4]([CH3:6])[CH2:3][CH2:2][O:20][C:18](=[O:19])[CH2:17][O:16][N:15]=[C:13]([CH3:14])[C:12]1[CH:21]=[CH:22][C:9]([Cl:8])=[CH:10][CH:11]=1

参加物

6

反応物 3

HCID 79012-Chloro-N,N-dimethylethylamineHCID 28212572-[1-(4-chlorophenyl)ethylideneamino]oxyacetic AcidHCID 5360545Sodium

生成物 1

HCID 85439121HCID 85439121、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

4.3 g of 2-chloro-N,N-dimethyl ethylamine was added to a suspension of 10 g of the sodium salt of (4-chloro-α -methylbenzylidene)amino-oxyacetic acid in 30 ml of dimethylformamide. The mixture was stirred for 72 hours. It was then diluted with water and extracted with diethylether. The resulting ethereal solution was extracted with 20 ml of 2N hydrochloric acid. The acid extract was then made basic with 30ml of 2N sodium hydroxide and extracted with diethylether. The latter ethereal extract was washed, dried over anhydrous sodium sulphate and after concentration by evaporation neutralized with alcoholic hydrochloric acid. When diethylether was added the hydrochloride of the (2-dimethyl-aminoethyl)ester of (4-chloro-α -methylbenzylidene) aminooxyacetic acid crystallized out. It was recrystallized from an alcohol-ether mixture; melting point 160° -162° C with decomposition.

後処理

  1. extractionextracted with diethylether
  2. extractionThe resulting ethereal solution was extracted with 20 ml of 2N hydrochloric acid
  3. extractionThe acid extract
  4. extractionextracted with diethylether
  5. extractionThe latter ethereal extract
  6. washwas washed
  7. dry with materialdried over anhydrous sodium sulphate
  8. concentrationafter concentration
  9. customby evaporation
  10. additionWhen diethylether was added the hydrochloride of the (2-dimethyl-aminoethyl)ester of (4-chloro-α -methylbenzylidene) aminooxyacetic acid
  11. customcrystallized out
  12. customIt was recrystallized from an alcohol-ether mixture

出典と根拠

ORDレコード
ord-d7024198808444cca8cf9a8917e129a7
出典データセット
uspto-grants-1977_08
特許番号
US04044023

反応ノート

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