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tert-Butoxy bis(dimethylamino)methane → HCID 53750001, 화합물

HRID 1708533
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HRID 1708533 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([Cl:9])=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11].C(O[CH:18](N(C)C)[N:19]([CH3:21])[CH3:20])(C)(C)C>O1CCCC1>[Cl:1][C:2]1[CH:7]=[C:6]([CH:8]=[CH:18][N:19]([CH3:21])[CH3:20])[C:5]([Cl:9])=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11]
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참가 물질

4

반응물 2

HCID 79885tert-Butoxy bis(dimethylamino)methaneHCID 2516781,4-Dichloro-2-methyl-5-nitrobenzene

생성물 1

HCID 53750001HCID 53750001, 화합물수율 58%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

2,5-Dichloro-4-methyl-nitrobenzene (50 g, 0.24 mol) was heated at reflux, in tetrahydrofuran (200 ml), with t-butoxy-bis(dimethylamino)methane (63.3 g, 0.364 mol) for 8 hours. The reaction mixture was cooled to room temperature and slowly poured into hexanes (3L) with stirring. The desired product was collected by filtration as a dark red solid, 36.9 g, 58% yield. mp 173°-5° C. NMR (CDCl3) δ 8.01 (s, 1), 7.32 (s, 1), 7.08 (d, 1), 5.27 (d, 1), 3.00 (s, 6). Analysis Calculated for C10H10N2O2Cl2 : C, 45.99; H, 3.86; N, 10.73, Found: C, 45.91; H, 3.72; N, 10.61.

후처리

  1. filtrationThe desired product was collected by filtration as a dark red solid, 36.9 g, 58% yield

출처 및 근거

ORD 기록
ord-905973fa2921471b9ab160931228501e
출처 데이터셋
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05359068

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