Bromine → 2-Amino-5-bromopyridine-3-carboxylic acid--hydrogen bromide (1/1)

HRID 1362100노트

반응식

HRID 1362100 반응식
[Br:1]Br.[NH2:3][C:4]1[N:12]=[CH:11][CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=[O:7]>C(O)(=O)C>[BrH:1].[NH2:3][C:4]1[N:12]=[CH:11][C:10]([Br:1])=[CH:9][C:5]=1[C:6]([OH:8])=[O:7]

참가 물질

4

반응물 2

HCID 24408Bromine2회HCID 729302-Aminonicotinic acid

생성물 1

HCID 573505542-Amino-5-bromopyridine-3-carboxylic acid--hydrogen bromide (1/1)수율 183.9%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Bromine (7.5 mL, 146 mmol) was added dropwise over 10 min to a suspension of 2-amino-nicotinic acid (20.0 g, 145 mmol) in glacial acetic acid (250 mL) cooled in an ice bath. After the bromine addition was complete, the mixture was stirred at ambient temperature for 2 d. The resulting light yellow solid was isolated by filtration, washed with Et2O, and dried under high vacuum (40° C.) for several hours to give the title compound (40.0 g, 93%): 1H NMR (300 MHz, DMSO-d6) δ 8.33 (d, J=2.5 Hz, 1H), 8.20 (d, J=2.5 Hz, 1H), 8.02 (bs, 3H); ESI MS m/e 217 (M+H)+.

후처리

  1. temperaturecooled in an ice bath
  2. customThe resulting light yellow solid was isolated by filtration
  3. washwashed with Et2O
  4. customdried under high vacuum (40° C.) for several hours

출처 및 근거

ORD 기록
ord-1a2c058611d147c59d84997afa6c5b1f
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07879872B2

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