Stannous chloride dihydrate → 4-Hydrazino-3-methoxybenzoic acid hydrochloride

HRID 565811

反応式

HRID 565811 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])=[CH:8][C:7]=1[O:15][CH3:16].O.O.[Cl:19][Sn]Cl>O.Cl>[ClH:19].[NH:5]([C:6]1[CH:14]=[CH:13][C:9]([C:10]([OH:12])=[O:11])=[CH:8][C:7]=1[O:15][CH3:16])[NH2:1]

参加物

6

反応物 3

HCID 61436Stannous chloride dihydrateHCID 2880572486-69-3HCID 23668193Sodium Nitrite

生成物 1

HCID 702454494-Hydrazino-3-methoxybenzoic acid hydrochloride

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
0 °C

実験手順

A solution of 2.17 g of NaNO2 in 40 ml of H2O is added slowly to a solution, cooled to 0° C., of 5 g of 4-amino-3-methoxybenzoic acid in 50 ml of concentrated HCl. After 1 hour 15 minutes of stirring at 0° C., the mixture is cooled to −10° C., and a solution of 23.6 g of SnCl2.2H2O in 20 ml of concentrated HCl and 20 ml of water is added over 30 min. After one and a half hours of stirring at −10° C., the mixture is filtered, and the precipitate is washed with 50 ml of pentane to obtain, after drying, 6 g of expected product.

後処理

  1. temperaturethe mixture is cooled to −10° C.
  2. stirringAfter one and a half hours of stirring at −10° C.
  3. filtrationthe mixture is filtered
  4. washthe precipitate is washed with 50 ml of pentane
  5. customto obtain
  6. customafter drying

出典と根拠

ORDレコード
ord-c12f759c91d64811887cbbb08345c3e3
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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