Stannous Chloride → HCID 67451538, 화합물

HRID 571092

반응식

HRID 571092 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 67451538HCID 67451538, 화합물

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매2회HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ac315b3b73a945a7bd623cb7712163ca
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09024041B2

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