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Benzoyl chloride → HCID 13406007, 화합물

HRID 1831044
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HRID 1831044 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([O:8][CH3:9])=[N:6][CH:7]=1.C(N(C(C)C)C(C)C)C.[C:19](Cl)(=[O:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.CCCCCCC>ClCCl>[CH3:9][O:8][C:5]1[N:6]=[CH:7][C:2]([NH:1][C:19](=[O:26])[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[CH:3][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 7412Benzoyl chlorideHCID 8900HeptaneHCID 811216-Methoxy-3-pyridinylamineHCID 81531Diisopropylethylamine

생성물 1

HCID 13406007HCID 13406007, 화합물수율 75.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 5-amino-2-methoxypyridine (2.48 g, 20.0 mmol) and N-ethyldiisopropylamine (2.84 g, 22.0 mmol) in dichloromethane (20 ml) was cooled in an ice-bath. Benzoyl chloride (3.09 g, 22 mmol) was slowly added by means of a syringe. The cooling bath was removed and stirring was continued at room temperature for 18 hours. Dichloromethane was added and the solution was extracted with water. The organic layer was dried over sodium sulphate, filtered and evaporated in vacuo leaving a dark solid. Crystallisation from ethyl acetate:heptane yielded the title compound (3.44 g, 75% yield).

후처리

  1. customThe cooling bath was removed
  2. additionDichloromethane was added
  3. extractionthe solution was extracted with water
  4. dry with materialThe organic layer was dried over sodium sulphate
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customleaving a dark solid
  8. customCrystallisation from ethyl acetate

출처 및 근거

ORD 기록
ord-964efa1bbc1f4adebf7cc109f7a505c0
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07067517B2

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