1-Bromooctane → HCID 20322535, 화합물

HRID 840003노트

반응식

HRID 840003 반응식
[K].[CH2:2]([C:4]1([CH3:20])[NH:15][C:14]([CH2:17][CH3:18])([CH3:16])[CH2:13][C:6]2([NH:10][C:9](=[O:11])[NH:8][C:7]2=[O:12])[CH:5]1[CH3:19])[CH3:3].[CH2:21](Br)[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]>CN(C)C=O>[CH2:2]([C:4]1([CH3:20])[NH:15][C:14]([CH2:17][CH3:18])([CH3:16])[CH2:13][C:6]2([NH:10][C:9](=[O:11])[N:8]([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:7]2=[O:12])[CH:5]1[CH3:19])[CH3:3]

참가 물질

5

반응물 3

HCID 81401-BromooctaneHCID 5462222PotassiumHCID 203401897,9-Diethyl-6,7,9-trimethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione2회

생성물 1

HCID 20322535HCID 20322535, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

To 70 ml of dimethylformamide were added 8 g of the potassium salt of 7,9-diethyl-6,7,9-trimethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione (Compound 1) and 5.2 g of octyl bromide; the mixture was heated, with stirring, at 60° C for 2 hours. The reaction mixture was then concentrated by evaporation under reduced pressure, and benzene was added to the residue. The resulting benzene solution was washed with water and then dried over magnesium sulphate. After removing the benzene, the resulting oily product was first purified by column chromatography on silica gel (eluent: benzene containing 5% of triethylamine) and then by recrystallization from hexane, giving 3.0 g of Compound 5, mp 65° - 67° C.

후처리

  1. temperaturethe mixture was heated
  2. concentrationThe reaction mixture was then concentrated by evaporation under reduced pressure, and benzene
  3. additionwas added to the residue
  4. washThe resulting benzene solution was washed with water
  5. dry with materialdried over magnesium sulphate
  6. customAfter removing the benzene
  7. customthe resulting oily product was first purified by column chromatography on silica gel (eluent: benzene containing 5% of triethylamine)
  8. customby recrystallization from hexane

출처 및 근거

ORD 기록
ord-a113adb3b1af40ceb38cfcd397f3a084
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04097587

반응 노트

불러오는 중…