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Hydrazine hydrate (1:1) → HCID 135504036, 화합물

HRID 2221085
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HRID 2221085 반응식
O.[NH2:2][NH2:3].Br[C:5]1[C:6](=[O:14])[NH:7][C:8]([N:11]([CH3:13])[CH3:12])=[N:9][N:10]=1>O>[CH3:12][N:11]([CH3:13])[C:8]1[NH:7][C:6](=[O:14])[C:5]([NH:2][NH2:3])=[N:10][N:9]=1
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 1354906346-Bromo-3-(dimethylamino)-1,2,4-triazin-5(2H)-one

생성물 1

HCID 135504036HCID 135504036, 화합물수율 63.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

With stirring, hydrazine monohydrate (1.44 ml, 30 mmol) was added at 25° C. to a solution of the bromide (X) (2.20 g, 10 mmol) in water (80 ml). The reaction mixture was heated to reflux, cooled to room temperature and, for crystallization, allowed to stand for several hours. The crystals were filtered off, washed with water and dried in the air, giving the hydrazine (XI) (1.08 g, 63%) as a white solid of melting point 264-266° C. (from ethanol): IR spectrum vmax (NaCl/nujol/cm−1) 3324s, 3301s, (NH), 1641s (C═O), 1575s, 1516s, 1397s, 1304w, 1260w, 1204w, 1165w, 1133w, 1068w, 1050s, 1005w, 923s, 833w, 786s, 709s, 683s; NMR spectrum: δH (270 MHz, DMSO-d6): 11.25 (2H, bs, NH2), 7.18 (1H, bs, NH), 2.96 (6H, s, NCH3);

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux
  3. waitto stand for several hours
  4. filtrationThe crystals were filtered off
  5. washwashed with water
  6. customdried in the air

출처 및 근거

ORD 기록
ord-6bf4083e483947d2a8d512d4440f1a4d
출처 데이터셋
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07368437B1

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