Acetic Acid → 3-Amino-6-chloropyridine-2-carbonitrile

HRID 1517427노트

반응식

HRID 1517427 반응식
[Cl:1][C:2]1[N:7]=[C:6]([C:8]#[N:9])[C:5]([N+:10]([O-])=O)=[CH:4][CH:3]=1.C(O)(=O)C.[O-]S(S([O-])=O)=O.[Na+].[Na+].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>O>[NH2:10][C:5]1[C:6]([C:8]#[N:9])=[N:7][C:2]([Cl:1])=[CH:3][CH:4]=1

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 14812Phosphorus oxide (P4O10)HCID 24489Sodium DithioniteHCID 133817056-Chloro-3-nitropyridine-2-carbonitrile

생성물 1

HCID 5927503-Amino-6-chloropyridine-2-carbonitrile수율 80.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a suspension of 6-chloro-3-nitro-pyridine-2-carbonitrile (5.5 g, 30 mmol) in water (100 ml), was added acetic acid (5.4 ml, 90 mmol). The mixture was stirred at room temperature for 20 minutes. Then, Na2S2O4 (20 g, 86%, 90 mmol) was added slowly. The reaction mixture was stirred at room temperature for another 2 hours. The precipitate was filtered off and washed with cold water (2×10 ml). The precipitate was dried over P2O5 yielding the title compound as a yellowish solid (3.7 g, yield: 80%) which was characterised as follows:

후처리

  1. stirringThe reaction mixture was stirred at room temperature for another 2 hours
  2. filtrationThe precipitate was filtered off
  3. washwashed with cold water (2×10 ml)

출처 및 근거

ORD 기록
ord-35e062a7687e45758a82e9a06f4508d2
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08232278B2

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