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Dimethylamine → HCID 11391437, 화합물

HRID 1991192
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HRID 1991192 반응식
[Cl:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][C:3]=1[S:11](Cl)(=[O:13])=[O:12].[CH3:15][NH:16][CH3:17].C(N(CC)CC)C>CO>[Cl:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][C:3]=1[S:11]([N:16]([CH3:17])[CH3:15])(=[O:13])=[O:12]
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참가 물질

5

반응물 3

HCID 674DimethylamineHCID 8471TriethylamineHCID 230424882-chloro-3-nitrobenzene-1-sulfonyl chloride

생성물 1

HCID 11391437HCID 11391437, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

2-Chloro-3-nitrobenzenesulfonyl chloride (235 mg, 0.918 mmol) was treated with a 2 M solution of dimethylamine in methanol (0.55 mL, 1.10 mmol), and triethylamine (0.13 mL, 0.918 mmol) in methanol (1 mL), and the suspension was stirred at room temperature for 2.5 h. The volatiles were removed in vacuo, and the residue was purified by column chromatography using heptane/ethyl acetate, 70:30-50:50 as an eluent, affording 2-chloro-N,N-dimethyl-3-nitrobenzenesulfonamide, 202 mg (83%) as a white solid. MS (ESI) m/z 265 [M+H]. 1H NMR (400 MHz, CDCl3) δ ppm 2.95 (s, 6 H); 7.56 (t, J=8.0 Hz, 1H), 7.88 (dd, J=8.1, 1.5 Hz, 1H), 8.31 (dd, J=8.1, 1.5 Hz, 1H).

후처리

  1. customThe volatiles were removed in vacuo
  2. customthe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-5927497239ed4c45af1671aeb12f3aee
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07645784B2

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