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3-Bromo-5-chloropyridin-2-amine → 3-Bromo-5-chloropyridin-2-ol

HRID 895884
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HRID 895884 반응식
N[C:2]1[C:7]([Br:8])=[CH:6][C:5]([Cl:9])=[CH:4][N:3]=1.N([O-])=[O:11].[Na+]>O.Cl>[Br:8][C:7]1[C:2](=[O:11])[NH:3][CH:4]=[C:5]([Cl:9])[CH:6]=1
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참가 물질

5

반응물 2

HCID 27639713-Bromo-5-chloropyridin-2-amineHCID 23668193Sodium Nitrite

생성물 1

HCID 27267913-Bromo-5-chloropyridin-2-ol수율 69%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매2회

실험 절차

A solution of 2-amino-3-bromo-5-chloropyridine (4.0 g, 19.3 mmol) in water (30 mL) and conc. HCl (5.2 mL) was cooled with an ice bath to 0° C. and was treated with a solution of sodium nitrite (1.33 g, 19.3 mmol) in water (12 mL) over 10 min. The mixture was stirred for an additonal 10 min and allowed to warm to room temperature over 48 hr. The mixture was filtered. The solids were washed with water, then with CCl4 and were dried under vacuum at 50° C. for 3 hr to give 3-bromo-5-chloro-1H-2-pyridone (2.77 g, 69%), mp 173.5-175° C.

후처리

  1. filtrationThe mixture was filtered
  2. washThe solids were washed with water
  3. dry with materialwith CCl4 and were dried under vacuum at 50° C. for 3 hr

출처 및 근거

ORD 기록
ord-b2917dd7b80e4ff69cc61f3d52649290
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06916933B2

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