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Acetic Acid → Methyl 1-allyl-6-methyl-2-(4'-chlorophenyl)-4-oxonicotinate

HRID 2107897
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인쇄 미리보기

반응식

HRID 2107897 반응식
[CH3:1][O:2][C:3]([C:5]1[C:10](=[O:11])[CH:9]=[C:8]([CH3:12])O[C:6]=1[C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][CH:14]=1)=[O:4].C(O)(=O)C.[CH2:24]([NH2:27])[CH:25]=[CH2:26].Cl>O.CO>[CH2:24]([N:27]1[C:8]([CH3:12])=[CH:9][C:10](=[O:11])[C:5]([C:3]([O:2][CH3:1])=[O:4])=[C:6]1[C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][CH:14]=1)[CH:25]=[CH2:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 7853AllylamineHCID 14075263HCID 14075263, 화합물

생성물 1

HCID 22159875Methyl 1-allyl-6-methyl-2-(4'-chlorophenyl)-4-oxonicotinate수율 87.7%

시약·촉매·용매 2

HCID 887Methanol용매
HCID 962
Water
용매
2회

실험 절차

10 gms of 3-methoxycarbonyl-6-methyl-2-(4'-chlorophenyl)-4-pyrone, 1.65 gms glacial acetic acid and 100 mls of methanol are mixed in 500 ml flask fitted with a magnetic stirring bar and sidearm additionl funnel. 6.15 gms of allylamine are slowly added (one hour addition time). Three hours later 20 mls of water and 8 mls of concentrate HCl are added. This reaction mixture is allowed to stand at room temperature for one hour, then is poured into 400 mls of water and extracted with methylene chloride (2×100 mls). Removal of the solvent yields 10 gms of crude methyl 1-allyl-6-methyl-2-(4'-chlorophenyl)-4-oxonicotinate.

후처리

  1. customfitted with a magnetic stirring bar and sidearm additionl funnel
  2. addition(one hour addition time)
  3. extractionextracted with methylene chloride (2×100 mls)
  4. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-816d146482e64ccc8c2158bdf5721daa
출처 데이터셋
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04936904

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