Water → HCID 21898026, 화합물

HRID 719239노트

반응식

HRID 719239 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-dimethylaminonapthalene-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-0c22dd35bbef40fe8b797dbfc6e42433
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07132429B2

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