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Hydrazine hydrate (1:1) → HCID 135504036、化合物

HRID 2221085
ノート
印刷プレビュー

反応式

HRID 2221085 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 135504036HCID 135504036、化合物収率 63.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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);

後処理

  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

出典と根拠

ORDレコード
ord-6bf4083e483947d2a8d512d4440f1a4d
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07368437B1

反応ノート

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