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Sulfuric Acid → HCID 72312730, 화합물

HRID 1161371
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인쇄 미리보기

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HRID 1161371 반응식
N1C(C)=CC(C)=CC=1C.Cl[C:11]([O:13][CH3:14])=[O:12].[CH3:15][S:16][C:17](=[NH:39])[C:18](=[N:30][C:31]1[CH:36]=[CH:35][C:34]([C:37]#[N:38])=[CH:33][CH:32]=1)[C:19]1[CH:24]=[C:23]([O:25][CH3:26])[CH:22]=[C:21]([O:27][CH3:28])[C:20]=1[F:29].S(=O)(=O)(O)O>C1(C)C=CC=CC=1.C(OCC)(=O)C>[CH3:14][O:13][C:11](=[O:12])[N:39]=[C:17]([S:16][CH3:15])[C:18](=[N:30][C:31]1[CH:36]=[CH:35][C:34]([C:37]#[N:38])=[CH:33][CH:32]=1)[C:19]1[CH:24]=[C:23]([O:25][CH3:26])[CH:22]=[C:21]([O:27][CH3:28])[C:20]=1[F:29]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 1118Sulfuric AcidHCID 6586Methyl chloroformateHCID 79532,4,6-TrimethylpyridineHCID 59517045HCID 59517045, 화합물

생성물 1

HCID 72312730HCID 72312730, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매
HCID 8857
Ethyl Acetate
용매

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온도
85 °C

실험 절차

After adding 2.97 ml of 2,4,6-collidine and 1.74 ml of methyl chloroformate to a solution of 2.01 g of 2-(4-cyanophenylimino)-2-(2-fluoro-3,5-dimethoxyphenyl)thioacetimidic acid methyl ester in 80 ml of toluene, the mixture was stirred at 85° C. for 20 hours under a nitrogen atmosphere. After cooling the reaction mixture, 400 ml of ethyl acetate and 200 ml of a 2% aqueous sulfuric acid solution were added and the organic layer was washed with 300 ml of water and 300 ml of saturated brine. The organic layer was dried over anhydrous magnesium sulfate, the desiccating agent was filtered off and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (heptane-ethyl acetate (3:2)) to give the title compound (1.89 g) as a light yellow solid.

후처리

  1. additionwere added
  2. washthe organic layer was washed with 300 ml of water and 300 ml of saturated brine
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. filtrationthe desiccating agent was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (heptane-ethyl acetate (3:2))

출처 및 근거

ORD 기록
ord-6bae17e8ab674faf90db9130a2221801
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07816522B2

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