3-Amino-2-naphthoic acid → 3-Hydrazino-2-naphthoic acid

HRID 1250756ノート

反応式

HRID 1250756 の反応式
[NH2:1][C:2]1[C:3]([C:12]([OH:14])=[O:13])=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.[N:15]([O-])=O.[Na+].Cl[Sn]Cl.O>Cl.O>[NH:1]([C:2]1[C:3]([C:12]([OH:14])=[O:13])=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2)[NH2:15]

参加物

6

反応物 3

HCID 222443-Amino-2-naphthoic acidHCID 23668193Sodium NitriteHCID 43835034Tin dichloride dihydrate

生成物 1

HCID 47388533-Hydrazino-2-naphthoic acid

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

実験手順

To 3-amino-2-naphthoic acid (15 g, 66.8 mmol) in conc. HCl (100 ml) and water (100 ml) at 0° C. was added NaNO2 (9.22 g, 69 mmol) in 1 g portions while maintaing the reaction temperature below 0° C. After 30 min below 0° C., SnCl2.H2O (75 g) was added in portions over 20 min. The ice bath was removed and stirred at ambient temperature for 1 h. Reaction was filtered and the filter cake washed with water and air dried. The crude material containing tin (II) salts was used as is and gave a mp>300° C.

後処理

  1. customthe reaction temperature below 0° C
  2. customThe ice bath was removed
  3. customReaction
  4. filtrationwas filtered
  5. washthe filter cake washed with water and air
  6. customdried
  7. additionThe crude material containing tin (II) salts
  8. customgave a mp>300° C.

出典と根拠

ORDレコード
ord-f4c874b2c8d844c2bc458194be95cd11
出典データセット
uspto-grants-2002_01
特許番号
US06339099B1

反応ノート

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