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Stannous chloride dihydrate → 6-Hydrazino-4-trifluoromethylquinolin-2(1H)-one

HRID 1063428
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HRID 1063428 반응식
[NH2:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=[O:12])[CH:6]=[C:5]2[C:13]([F:16])([F:15])[F:14].[N:17]([O-])=O.[Na+].O.O.Cl[Sn]Cl>Cl.O>[NH:1]([C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=[O:12])[CH:6]=[C:5]2[C:13]([F:16])([F:14])[F:15])[NH2:17]
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참가 물질

6

반응물 3

HCID 61436Stannous chloride dihydrateHCID 160903086-amino-4-trifluoromethylquinolin-2(1H)-oneHCID 23668193Sodium Nitrite

생성물 1

HCID 98995846-Hydrazino-4-trifluoromethylquinolin-2(1H)-one

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매2회HCID 962Water
용매

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온도
-1 °C

실험 절차

In a 250 mL rb flask a suspension of Compound 200 (structure 3 of Scheme XXXIII) (2.28 g, 10 mmol) in 10 mL conc. HCl was cooled to −1° C. and a solution of NaNO2 (0.40 g, 12 mmol) in water (5 mL) was added dropwise in 20 min. The dark yellow suspension was stirred at −1° C. for 1 h and then a solution of SnCl2.2H2O (5.2 g, 15 mmol) in conc HCl (10 mL) was added dropwise in 10 min. The light yellow suspension of Compound 793 was stirred at −1° C. for 2 h and then used directly or kept in a refrigerator at −1° C. until it was used (the crude compound can be stored for at least one month without decomposition).

후처리

  1. stirringwas stirred at −1° C. for 2 h
  2. customkept in a refrigerator at −1° C. until it
  3. waitcan be stored for at least one month without decomposition

출처 및 근거

ORD 기록
ord-b44c63f02f3f41109c3b7e003f4a3315
출처 데이터셋
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06964973B2

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