5-Amino-2-chlorobenzoic acid → 2-Chloro-5-hydrazinylbenzoic acid hydrochloride

HRID 1585281

反応式

HRID 1585281 の反応式
[N:1]([O-])=O.[Na+].[NH2:5][C:6]1[CH:7]=[CH:8][C:9]([Cl:15])=[C:10]([CH:14]=1)[C:11]([OH:13])=[O:12].O.O.Cl[Sn]Cl>O.Cl>[ClH:15].[NH:5]([C:6]1[CH:7]=[CH:8][C:9]([Cl:15])=[C:10]([CH:14]=1)[C:11]([OH:13])=[O:12])[NH2:1]

参加物

6

反応物 3

HCID 378795-Amino-2-chlorobenzoic acidHCID 61436Stannous chloride dihydrateHCID 23668193Sodium Nitrite

生成物 1

HCID 164957252-Chloro-5-hydrazinylbenzoic acid hydrochloride収率 123.1%

試薬・触媒・溶媒 2

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

反応条件

温度
-3 °C

実験手順

A solution of 2.11 g of NaNO2 in 40 ml of water is added over 30 minutes to a suspension, cooled to -2° C., of 5 g of 5-amino-2-chlorobenzoic acid in 50 ml of concentrated HCl. The solution is stirred for 2 hours at -3° C. and cooled to -10° C., and a solution of 23 g of SnCl2.2H2O in 20 ml of concentrated HCl and 20 ml of water is added over 30 minutes. The mixture is stirred for one and a half hours at 0° C. and filtered, and the precipitate is dried to obtain 4 g of expected product.

後処理

  1. temperaturecooled to -10° C.
  2. stirringThe mixture is stirred for one and a half hours at 0° C.
  3. filtrationfiltered
  4. customthe precipitate is dried

出典と根拠

ORDレコード
ord-b6b3f72446f84a7f876fc3ec875f63e3
出典データセット
uspto-grants-1999_08
特許番号
US05936123

関連ノート

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