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Iodoethane → Ethyl 2,4-dibromo-3-ethoxybenzoate

HRID 2257495
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HRID 2257495 반응식
[Br:1][C:2]1[C:12]([OH:13])=[C:11]([Br:14])[CH:10]=[CH:9][C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5].C(=O)([O-])[O-].[K+].[K+].I[CH2:22][CH3:23]>CN(C)C=O>[Br:1][C:2]1[C:12]([O:13][CH2:22][CH3:23])=[C:11]([Br:14])[CH:10]=[CH:9][C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 14851207Ethyl 2,4-dibromo-3-hydroxybenzoate

생성물 1

HCID 22621032Ethyl 2,4-dibromo-3-ethoxybenzoate수율 95.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
85 °C

실험 절차

Ethyl 2,4-dibromo-3-hydroxybenzoate (50 g) was added to a stirred suspension of potassium carbonate (106.4 g) in dry N,N-dimethylformamide (DMF). A solution of iodoethane (25.7 g) in DMF was added over 18 minutes, and the resulting mixture was heated at 85° C. for 1.3 hours. The cooled mixture was poured onto water and extracted with ether. The extract was washed (brine solution), dried (anhydrous magnesium sulphate) and the solvent evaporated in vacuo to give ethyl 2,4-dibromo-3-ethoxybenzoate (52.08 g), NMR 1.4(t,3H), 1.5(t,3H), 4.1(q,2H), 4.4(q,2H), 7.35(d,1H), 7.55(d,1H).

후처리

  1. additionThe cooled mixture was poured onto water
  2. extractionextracted with ether
  3. washThe extract was washed (brine solution)
  4. dry with materialdried (anhydrous magnesium sulphate)
  5. customthe solvent evaporated in vacuo

출처 및 근거

ORD 기록
ord-42a8bd8de0e0498ea66daaf5feddf49c
출처 데이터셋
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05658858

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