6-Methyl-5-nitropyridin-2-amine → HCID 178433443, 화합물

HRID 363321

반응식

HRID 363321 반응식
N[C:2]1[N:7]=[C:6]([CH3:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][CH:3]=1.N([O-])=[O:13].[Na+]>O>[OH:13][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 2479766-Methyl-5-nitropyridin-2-amineHCID 23668193Sodium Nitrite

생성물 1

HCID 178433443HCID 178433443, 화합물수율 80%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

A suspension of 3.0 gm (19.6 mMol) 6-amino-3-nitro-2-picoline in 50 mL water containing 3.5 mL concentrated sulfuric acid was heated to effect solution. The resultant solution was cooled to 0° C. and a solution of 2.0 gm (29.4 mMol) sodium nitrite in 10 mL water was added with vigorous stirring at a rate to maintain the reaction mixture ≤10° C. After 4 hours the reaction mixture was filtered. The solid was washed with water and dried under reduced pressure to provide 2.4 gm (80%) of the desired compound as a pale yellow solid.

후처리

  1. temperaturewas heated
  2. temperatureto maintain the reaction mixture ≤10° C
  3. filtrationAfter 4 hours the reaction mixture was filtered
  4. washThe solid was washed with water
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-9d92017cd9a543b2af904d7ec9737b75
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05874427

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