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Methanol → HCID 13084138, 화합물

HRID 543042
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HRID 543042 반응식
[CH3:1]O.S(Cl)(Cl)=O.[I:7][C:8]1[CH:13]=[CH:12][C:11]([N:14]2[C:19]([CH3:20])=[CH:18][C:17](=[O:21])[C:16]([C:22]([OH:24])=[O:23])=[N:15]2)=[CH:10][CH:9]=1.O>C(Cl)(Cl)Cl>[I:7][C:8]1[CH:13]=[CH:12][C:11]([N:14]2[C:19]([CH3:20])=[CH:18][C:17](=[O:21])[C:16]([C:22]([O:24][CH3:1])=[O:23])=[N:15]2)=[CH:10][CH:9]=1
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참가 물질

6

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HCID 887MethanolHCID 962WaterHCID 24386Thionyl ChlorideHCID 130841151-(4-Iodophenyl)-1,4-dihydro-4-oxo-6-methylpyridazine-3-carboxylic acid

생성물 1

HCID 13084138HCID 13084138, 화합물수율 47%

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
0 °C

실험 절차

To 50 ml of methanol, cooled to -5°, there is added dropwise 2.62 g (0.022 mol) of thionyl chloride (pot temperature maintained between -5° C. and 0° C.). The solution is stirred at 0° C. for 15 min and to it there is added 7.12 g (0.02 mol) of 1-(4-iodophenyl)-1,4-dihydro-4-oxo-6-methylpyridazine-3-carboxylic acid. (See Example 3). The suspension formed is stirred at room temperature for 3 days and to it there is added 200 ml of water. The suspension that forms is stirred at room temperature for 2 days and is vacuum filtered. The filter cake is air dried to afford 4 g of crude product. The crude product is suspended in 25 ml of chloroform and filtered. The filtrate is concentrated in vacuo to afford 3.5 g (47% yield) of product, mp 185°-187° C.

후처리

  1. customThe suspension formed
  2. stirringis stirred at room temperature for 3 days and to it there
  3. stirringThe suspension that forms is stirred at room temperature for 2 days
  4. filtrationfiltered
  5. customdried
  6. customto afford 4 g of crude product
  7. filtrationfiltered
  8. concentrationThe filtrate is concentrated in vacuo

출처 및 근거

ORD 기록
ord-2baaa7ee79554bfebae38400fc24a69f
출처 데이터셋
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04661145

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