4-Nitrobenzenesulfonyl chloride → HCID 874568, 화합물

HRID 624231노트

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HRID 624231 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10](Cl)(=[O:12])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].C(N(C(C)C)CC)(C)C.[CH3:23][CH:24]([CH3:28])[CH2:25][CH2:26][NH2:27]>ClCCl.C(=O)(O)[O-].[Na+]>[CH2:26]([NH:27][S:10]([C:7]1[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1)(=[O:12])=[O:11])[CH2:25][CH:24]([CH3:28])[CH3:23]

참가 물질

6

반응물 3

HCID 74044-Nitrobenzenesulfonyl chlorideHCID 7894IsoamylamineHCID 81531Diisopropylethylamine

생성물 1

HCID 874568HCID 874568, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 516892Sodium Bicarbonate용매

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온도
0 °C

실험 절차

4-Nitrobenzene-1-sulfonyl chloride (1.5 g, 6.57 mmol) was dissolved in dichloromethane (30 ml) and cooled to 0° C. followed by addition of diisopropylethylamine (2.293 ml, 13.13 mmol). 3-Methylbutan-1-amine (0.926 ml, 7.88 mmol) was dissolved in 5 ml dichloromethane and added via syringe. After the addition, the mixture was allowed to warm to room temperature for 3 hours. The solution was diluted with aqueous sodium bicarbonate and extracted twice with dichloromethane. The organics were combined, dried over magnesium sulfate, filtered and concentrated. Chromatography provided the title compound.

후처리

  1. additionadded via syringe
  2. additionAfter the addition
  3. temperatureto warm to room temperature for 3 hours
  4. extractionextracted twice with dichloromethane
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d0c461296de4417fb3d1e87938df67cf
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09302989B2

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