Stannous Chloride → HCID 67451538、化合物

HRID 571092

反応式

HRID 571092 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([O:11][CH3:12])[CH:3]=1.[N:13]([O-])=O.[Na+].[Sn](Cl)[Cl:18]>Cl.O>[ClH:18].[CH3:12][O:11][C:4]1[CH:3]=[C:2]([NH:1][NH2:13])[CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=[O:7]

参加物

6

反応物 3

HCID 24479Stannous ChlorideHCID 755994-Amino-o-anisic acidHCID 23668193Sodium Nitrite

生成物 1

HCID 67451538HCID 67451538、化合物

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒2 回HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

To a suspension of 4-amino-2-methoxybenzoic acid (3.00 g, 18.0 mmol) in hydrochoric acid (1.0 M, 30 mL) at 0° C. was added a solution of sodium nitrite (1.28 g, 18.5 mmol) in water (5.0 mL) over 5 min. The reaction mixture was maintained at 0° C. for 5 hr and was then treated with tin(II) chloride (9.53 g, 50.3 mmol) in hydrochloric acid (1M, 60 mL) and warmed to RT for 64 hr. A thick precipitate formed which was isolated by filtration, washed with water (50 mL) and ether (15 mL) and dried in vacuo to afford 2-methoxy-4-hydrazinylbenzoic acid hydrochloride as a beige solid (1.05 g, 90% purity, 24%); Rt 0.17 min (Method 2); m/z 181 (M+H)+, (ES+). This material was used in the subsequent step without further purification.

後処理

  1. temperaturewarmed to RT for 64 hr
  2. customA thick precipitate formed which
  3. customwas isolated by filtration
  4. washwashed with water (50 mL) and ether (15 mL)
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-ac315b3b73a945a7bd623cb7712163ca
出典データセット
uspto-grants-2015_05
特許番号
US09024041B2

関連ノート

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