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Methanesulfonamide → 2-Methyl-1-(methylsulphonylaminocarbonyl)-5-nitrobenzene

HRID 2379356
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반응식

HRID 2379356 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4](O)=[O:5].[CH3:14][S:15]([NH2:18])(=[O:17])=[O:16].Cl.CN(C)CCCN=C=NCC>CN(C)C1C=CN=CC=1.ClCCl>[CH3:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([NH:18][S:15]([CH3:14])(=[O:17])=[O:16])=[O:5]
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참가 물질

6

반응물 3

HCID 72879MethanesulfonamideHCID 5196832-Methyl-5-nitrobenzoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

생성물 1

HCID 189577932-Methyl-1-(methylsulphonylaminocarbonyl)-5-nitrobenzene수율 79.5%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매
HCID 6344
Dichloromethane
용매

실험 절차

The title compound was prepared in the same way as that described in Example 11, Step 1, using 2-methyl-5-nitrobenzoic acid (5 g, 27.6 mmol), methyl sulphonamide (2.63 g, 27.6 mmol), 4-dimethylaminopyridine (3.37 g, 27.6 mmol), 1-[3-(dimethylamino)propyl]-3-ethyl carbodiimide hydrochloride (5.29 g, 27.6 mmol) and anhydrous dichloromethane (200 ml). The title compound (5.67 g, 79%) was afforded as a colourless solid. mp 180° C. (dec.). 1H NMR (360 MHz, D6-DMSO) δ 2.50 (3H, s), 3.42 (3H, s), 7.61 (1H, d, J=8.5 Hz), 8.28 (1H, dd, J=8.4 and 2.5 Hz), 8.36 (1H, d, J=2.5 Hz), 12.46 (1H, brs).

후처리

  1. customThe title compound was prepared in the same way as

출처 및 근거

ORD 기록
ord-3c2bfdf002aa44be99bc544251dba7af
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05360802

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