Diethylamine → N,N-diethyl-4-iodobenzamide

HRID 747109

反応式

HRID 747109 の反応式
[I:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][CH:3]=1.[CH3:11][CH2:12][N:13](CC)[CH2:14][CH3:15].N(CC)CC>C(Cl)Cl>[I:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([N:13]([CH2:14][CH3:15])[CH2:12][CH3:11])=[O:7])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 8021DiethylamineHCID 8471TriethylamineHCID 743734-Iodobenzoyl chloride

生成物 1

HCID 875218N,N-diethyl-4-iodobenzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a mixture of 4-iodo-benzoyl chloride (75 g) in 500 mL CH2Cl2 was added a mixture of Et3N (50 mL) and Et2NH (100 mL) at 0° C. After the addition, the resulting reaction mixture was warmed up to room temperature in 1 hr and was then washed with saturated ammonium chloride. The organic extract was dried (Na2SO4), filtered and concentrated. Residue was recrystallized from hot hexanes to give 80 g of INTERMEDIATE 5.

後処理

  1. additionwas added
  2. additionAfter the addition
  3. customthe resulting reaction mixture
  4. washwas then washed with saturated ammonium chloride
  5. extractionThe organic extract
  6. dry with materialwas dried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customResidue was recrystallized from hot hexanes

出典と根拠

ORDレコード
ord-28b78c804afd448ea22a9636a4b3cf3b
出典データセット
uspto-grants-2008_07
特許番号
US07396834B2

関連ノート

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