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Diethylamine → N,N-diethyl-4-iodobenzamide

HRID 747109
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HRID 747109 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8021DiethylamineHCID 8471TriethylamineHCID 743734-Iodobenzoyl chloride

생성물 1

HCID 875218N,N-diethyl-4-iodobenzamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-28b78c804afd448ea22a9636a4b3cf3b
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07396834B2

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