Dichloromethane → 2-nitro-N-(2-pyridin-3-ylethyl)benzenesulfonamide

HRID 68998

반응식

HRID 68998 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10](Cl)(=[O:12])=[O:11])([O-:3])=[O:2].ClCCl.[NH2:17][CH2:18][CH2:19][C:20]1[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=1.C(N(CC)CC)C>O>[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10]([NH:17][CH2:18][CH2:19][C:20]1[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=1)(=[O:12])=[O:11])([O-:3])=[O:2]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 155402-Nitrobenzenesulfonyl chlorideHCID 8540512-(Pyridin-3-yl)ethan-1-amine

생성물 1

HCID 465565342-nitro-N-(2-pyridin-3-ylethyl)benzenesulfonamide수율 32.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2-Nitrobenzene sulfonyl chloride (11.64 g) was added to a dichloromethane solution (100 ml) of 3-(2-aminoethyl)pyridine (6.11 g) and triethylamine (9 ml) at 0° C. The mixture was stirred at room temperature for 2 hours. Water was added to the reaction mixture, followed by extraction with dichloromethane. The organic layer was dried with anhydrous sodium sulfate, and condensed under reduced pressure. The residue was crystallized from ethyl acetate to give the title compound (5.06 g) as a yellow powder.

후처리

  1. extractionfollowed by extraction with dichloromethane
  2. dry with materialThe organic layer was dried with anhydrous sodium sulfate, and condensed under reduced pressure
  3. customThe residue was crystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-c3ccd1da4a8f4ca2bfbf69713a3fb167
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822453B2

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