Iodoethane → HCID 21912331, 화합물

HRID 967997노트

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HRID 967997 반응식
Br[C:2]1[CH:22]=[C:21]([CH3:23])[C:5]([O:6][C:7]2[C:12]([CH3:13])=[C:11]([NH:14][CH:15]([CH2:18][CH3:19])[CH2:16][CH3:17])[CH:10]=[C:9]([CH3:20])[N:8]=2)=[C:4]([CH3:24])[CH:3]=1.[CH2:25](I)[CH3:26]>C1COCC1>[CH2:25]([C:2]1[CH:22]=[C:21]([CH3:23])[C:5]([O:6][C:7]2[C:12]([CH3:13])=[C:11]([NH:14][CH:15]([CH2:18][CH3:19])[CH2:16][CH3:17])[CH:10]=[C:9]([CH3:20])[N:8]=2)=[C:4]([CH3:24])[CH:3]=1)[CH3:26]

참가 물질

4

반응물 2

HCID 6340IodoethaneHCID 21912379HCID 21912379, 화합물

생성물 1

HCID 21912331HCID 21912331, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
-78 °C

실험 절차

To a solution of [2-(4-bromo-2,6-dimethyl-phenoxy)-3,6-dimethyl-pyridin-4-yl]-(1-ethyl-propyl)-amine in dry THF was added n-butylithium at −78° C. After stirring at −78° C. for 10 min, ethyl iodide was added and the resulting mixture was stirred at −78° C. for 30 min, the dry-ice bath was removed. After stirring for 5 min, the mixture was quenched with brine and extracted with ethyl acetate. The organic layer was separated, dried, and concentrated to dryness. The residue was purified through silica gel chromatography to give the title compound. 1H NMR(CDCl3) d 6.89(s, 2H), 6.07(s, 1H), 3.72(d, 1H), 3.34(m, 1H), 2.58(q, 2H), 2.16(s, 3H), 2.12(s, 3H), 2.09(s, 6H), 1.4-1.7(m, 4H), 1.25(t, 3H), 0.96(t, 6H) ppm.

후처리

  1. stirringthe resulting mixture was stirred at −78° C. for 30 min
  2. customthe dry-ice bath was removed
  3. stirringAfter stirring for 5 min
  4. customthe mixture was quenched with brine
  5. extractionextracted with ethyl acetate
  6. customThe organic layer was separated
  7. customdried
  8. concentrationconcentrated to dryness
  9. customThe residue was purified through silica gel chromatography

출처 및 근거

ORD 기록
ord-453cc9a2b2c140bcb8901c2c90a5a8d6
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06956047B1

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