Stannous chloride dihydrate → 2,3-Dimethyl-4-hydrazinobenzoic acid hydrochloride

HRID 565810

反応式

HRID 565810 の反応式
[N:1]([O-])=O.[Na+].[NH2:5][C:6]1[CH:14]=[CH:13][C:9]([C:10]([OH:12])=[O:11])=[C:8]([CH3:15])[C:7]=1[CH3:16].O.O.[Cl:19][Sn]Cl>O.Cl>[ClH:19].[CH3:15][C:8]1[C:7]([CH3:16])=[C:6]([NH:5][NH2:1])[CH:14]=[CH:13][C:9]=1[C:10]([OH:12])=[O:11]

参加物

6

反応物 3

HCID 61436Stannous chloride dihydrateHCID 27627774-Amino-2,3-dimethylbenzoic acidHCID 23668193Sodium Nitrite

生成物 1

HCID 702445822,3-Dimethyl-4-hydrazinobenzoic acid hydrochloride収率 93.7%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒2 回HCID 962Water溶媒

反応条件

温度
-5 °C

実験手順

A solution of 1.87 g of NaNO2 in 7 ml of water is added slowly to a solution, cooled to −5° C., of 4.5 g of 4-amino-2,3-dimethylbenzoic acid in 135 ml of concentrated HCl . After 2 hours of stirring at −5° C., a solution of 25 g of SnCl2.2H2O in 250 ml of concentrated HCl is added at −10° C., and the mixture is stirred for 30 minutes at −5° C. and then 2 hours at RT. The mixture is filtered, and the precipitate is washed with 5 ml of concentrated HCl and dried under a stream of dry nitrogen and then under vacuum to obtain 5.5 g of expected product.

後処理

  1. stirringthe mixture is stirred for 30 minutes at −5° C.
  2. custom2 hours
  3. customat RT
  4. filtrationThe mixture is filtered
  5. washthe precipitate is washed with 5 ml of concentrated HCl
  6. customdried under a stream of dry nitrogen

出典と根拠

ORDレコード
ord-4fe7e2680d3d484683d1dbbd203dc0ff
出典データセット
uspto-grants-2001_01
特許番号
US06172239B2

関連ノート

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