Water → HCID 21898026, 화합물

HRID 1840854노트

반응식

HRID 1840854 반응식
[CH2:1]([NH2:12])[CH2:2][CH2:3][O:4][CH2:5][CH2:6][O:7][CH2:8][CH2:9][CH2:10][NH2:11].[S:13](Cl)([C:16]1[C:28]2[CH:27]=[CH:26][CH:25]=[C:21]([N:22]([CH3:24])[CH3:23])[C:20]=2[CH:19]=[CH:18][CH:17]=1)(=[O:15])=[O:14].O>C(#N)C>[NH2:11][CH2:10][CH2:9][CH2:8][O:7][CH2:6][CH2:5][O:4][CH2:3][CH2:2][CH2:1][NH:12][S:13]([C:16]1[C:28]2[C:20](=[C:21]([N:22]([CH3:24])[CH3:23])[CH:25]=[CH:26][CH:27]=2)[CH:19]=[CH:18][CH:17]=1)(=[O:15])=[O:14]

참가 물질

5

반응물 3

HCID 962WaterHCID 11801Dansyl chlorideHCID 763421-Propanamine, 3,3'-[1,2-ethanediylbis(oxy)]bis-

생성물 1

HCID 21898026HCID 21898026, 화합물수율 60.7%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

4,7-Dioxadecane-1,10-diamine (32.6 g, 0.185 mole) in acetonitrile (100 mL) was chilled in an ice bath. To this was slowly added dropwise dansyl chloride (5 g, 0.0185 mole) dissolved in acetonitrile (60 mL) over a 20 min. period. Stirring in an ice bath was continued for 1.5 hr. The reaction mixture was poured into water (about 300 mL) and extracted with dichloromethane (2×100 mL). The combined extracts were washed with water and dried to give an oil. The oil was purified by column chromatography (silica gel eluting with acetonitrile containing increasing amounts of ethanol) to provide 4.6 g of N-(10-amino-4,7-dioxadecyl)-5-dimethylaminonaphthalene-1-sulfonamide as a viscous oil.

후처리

  1. extractionextracted with dichloromethane (2×100 mL)
  2. washThe combined extracts were washed with water
  3. customdried
  4. customto give an oil
  5. customThe oil was purified by column chromatography (silica gel eluting with acetonitrile containing increasing amounts of ethanol)

출처 및 근거

ORD 기록
ord-dffe45500d174e46b338246eae4c514a
출처 데이터셋
uspto-grants-2004_01
특허 번호
US06683088B2

반응 노트

불러오는 중…