Stannous chloride dihydrate → 1-(4-Hydrazinobenzyl)-4-methylpiperazine

HRID 501221

反応式

HRID 501221 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:15]=[CH:14][C:12]([NH2:13])=[CH:11][CH:10]=2)[CH2:4][CH2:3]1.[N:16]([O-])=O.[Na+].O.O.Cl[Sn]Cl>C(O)(=O)C.O.Cl>[NH:13]([C:12]1[CH:14]=[CH:15][C:9]([CH2:8][N:5]2[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]2)=[CH:10][CH:11]=1)[NH2:16]

参加物

7

反応物 3

HCID 61436Stannous chloride dihydrateHCID 31539964-((4-Methylpiperazin-1-yl)methyl)anilineHCID 23668193Sodium Nitrite

生成物 1

HCID 684652221-(4-Hydrazinobenzyl)-4-methylpiperazine収率 99.1%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 313Hydrochloric Acid溶媒2 回HCID 962Water溶媒

実験手順

To a stirred solution of 4-[(4-methylpiperazin-1-yl)methyl]aniline (3.2 g, 15.57 mmol) in acetic acid: concentrated HCl (32:32 mL) at 10° C. was added NaNO2 (1.30 g, 18.78 mmol) in water (16 mL) and stirred for 10 min. Freshly prepared SnCl2.2H2O (11.75 g, 51.97 mmol) in concentrated HCl (32 mL) was added at 10° C. The temperature of the reaction mixture was allowed to rise to room temperature and maintained there for 4 hr. After filtering the reaction mixture, the precipitate was washed with water and the solid obtained was dried under reduced pressure to obtain 1-(4-hydrazinobenzyl)-4-methylpiperazine (3.4 g). 1H NMR (CD3OD, 200 MHz) δ: 7.66 (2H, d, J=8.4 Hz), 7.13 (2H, d, J=8.4 Hz), 4.46 (2H, s), 3.72 (8H, bm), 3.11 (3H, s);

後処理

  1. customto rise to room temperature
  2. temperaturemaintained there for 4 hr
  3. filtrationAfter filtering the reaction mixture
  4. washthe precipitate was washed with water
  5. customthe solid obtained
  6. customwas dried under reduced pressure

出典と根拠

ORDレコード
ord-09f2e740fd884df3b87df1985fce89cf
出典データセット
uspto-grants-2010_08
特許番号
US07772245B2

関連ノート

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