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

HRID 1768119노트

반응식

HRID 1768119 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 47388533-Hydrazino-2-naphthoic acid

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-294533f4f9ad41ec97fef4769847ca7b
출처 데이터셋
uspto-grants-2007_06
특허 번호
US07235575B2

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