Hydrochloric Acid → N-[(2,4-difluorophenyl)methyl]-N-hexyl-2,2-dimethylpentanamide

HRID 974402

反応式

HRID 974402 の反応式
[CH2:1]([NH:7][CH2:8][C:9]1[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:10]=1[F:16])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].C(N(CC)CC)C.[CH3:24][C:25]([CH3:32])([CH2:29][CH2:30][CH3:31])[C:26](Cl)=[O:27].Cl>C(OCC)C>[F:16][C:10]1[CH:11]=[C:12]([F:15])[CH:13]=[CH:14][C:9]=1[CH2:8][N:7]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[C:26](=[O:27])[C:25]([CH3:32])([CH3:24])[CH2:29][CH2:30][CH3:31]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 5191712,2-Dimethylvaleroyl chlorideHCID 19986431N-Hexyl-2,4-difluorobenzylamine

生成物 1

HCID 19986408N-[(2,4-difluorophenyl)methyl]-N-hexyl-2,2-dimethylpentanamide

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

22.7 g (0.10 mol) of N-hexyl-2,4-difluorobenzylamine and 24.3 g (0.24 mol) of triethylamine are dissolved in 150 ml of diethyl ether. A solution of 17.8 g (0.12 mol) of 2,2-dimethylpentanoyl chloride in 50 ml of diethyl ether is added dropwise at room temperature over the course of 30 minutes. The mixture is stirred for a further 18 hours at room temperature until the reaction is complete (GC check). For work-up, the resultant suspension is adjusted to pH 7 using 70 ml of 2N hydrochloric acid. Everything dissolves, and two phases form, which are separated. The organic phase is washed with 50 ml of water, dried using magnesium sulfate, filtered and evaporated on a vacuum rotary evaporator. 37.8 g of a pale yellow liquid, which is subjected to fractional distillation, are obtained. 21.4 g (63% of theory) of a colourless oil which boils at 126°-127° C. and 0.4 mbar are obtained.

後処理

  1. dissolutionEverything dissolves
  2. customtwo phases form, which are separated
  3. washThe organic phase is washed with 50 ml of water
  4. customdried
  5. filtrationfiltered
  6. customevaporated on a vacuum rotary evaporator
  7. distillation37.8 g of a pale yellow liquid, which is subjected to fractional distillation
  8. customare obtained
  9. custom21.4 g (63% of theory) of a colourless oil which boils at 126°-127° C. and 0.4 mbar are obtained

出典と根拠

ORDレコード
ord-fe2b8316ba6441fdaffddef32041f8b6
出典データセット
uspto-grants-1991_11
特許番号
US05068371

関連ノート

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