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Hydrochloric Acid → N1-(2,4-Difluorobenzyl)-3-Chloro-2,2-Dimethylpropanamide

HRID 974399
ノート
印刷プレビュー

反応式

HRID 974399 の反応式
[F:1][C:2]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:3]=1[CH2:4][NH2:5].N1C=CC=CC=1.[Cl:17][CH2:18][C:19]([CH3:24])([CH3:23])[C:20](Cl)=[O:21].Cl>C1(C)C=CC=CC=1>[Cl:17][CH2:18][C:19]([CH3:24])([CH3:23])[C:20]([NH:5][CH2:4][C:3]1[CH:6]=[CH:7][C:8]([F:10])=[CH:9][C:2]=1[F:1])=[O:21]
参加物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 313Hydrochloric AcidHCID 1049PyridineHCID 613453-Chloro-2,2-dimethylpropanoyl chlorideHCID 27332442,4-Difluorobenzylamine

生成物 1

HCID 2779689N1-(2,4-Difluorobenzyl)-3-Chloro-2,2-Dimethylpropanamide

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

28.6 g (0.20 mol) of 2,4-difluorobenzylamine and 19.0 g (0.24 mol) of pyridine are dissolved in 100 ml of toluene. 34.1 g (0.22 mol) of chloropivaloyl chloride are added dropwise to this solution at 20°-25° C. over the course of 15 minutes with ice-bath cooling. A suspension forms and is stirred for a further 3 hours at room temperature until the reaction is complete (GC check). For work-up, the pH is adjusted to between 1 and 2 using 50 ml of 2N hydrochloric acid. The white emulsion produced is extracted three times with 100 ml of toluene. The extract is washed with 100 ml of water, dried using magnesium sulfate and evaporated on a vacuum rotary evaporator. 49.2 g (94% of theory) of a yellow oil are obtained.

後処理

  1. temperaturecooling
  2. customThe white emulsion produced
  3. extractionis extracted three times with 100 ml of toluene
  4. washThe extract is washed with 100 ml of water
  5. customdried
  6. customevaporated on a vacuum rotary evaporator
  7. custom49.2 g (94% of theory) of a yellow oil are obtained

出典と根拠

ORDレコード
ord-fc63af1e980343348e0addb8c65b36a5
出典データセット
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05068371

反応ノート

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