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Hydrochloric Acid → HCID 20164696, 화합물

HRID 255840
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HRID 255840 반응식
C([O:3][C:4]([C:6]([CH:14]([CH2:23][C:24]#[CH:25])[C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:16]=1[Cl:22])([C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)[OH:7])=[CH2:5])C.Cl>CO>[Cl:22][C:16]1[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=1[CH:14]([CH2:23][C:24]#[CH:25])[C:6]([OH:7])([C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)[C:4](=[O:3])[CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 20164645HCID 20164645, 화합물

생성물 1

HCID 20164696HCID 20164696, 화합물수율 97.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 2.0 g of α-(1-ethoxyvinyl)-α-[2,4-dichloro-α-(2-propynyl)-benzyl]-3-pyridinemethanol (see Example 3, 1st end product), 1 ml of concentrated hydrochloric acid and 15 ml of methanol as a clear yellow solution is held at room temperature for 1 hour. Thereafter, the mixture is evaporated under reduced pressure in order to remove methanol and the residue is neutralized with saturated aqueous sodium bicarbonate solution. The aqueous mixture is extracted with ethyl acetate and the organic phase is washed with saturated aqueous sodium chloride solution and evaporated. Finally, the residue is recrystallized from methylene chloride/n-hexane. There are obtained 1.8 g of 4-(2,4-dichlorophenyl)-3-hydroxy-3-(3-pyridyl)-6-heptyn-2-one, m.p. 132° C.

후처리

  1. customThereafter, the mixture is evaporated under reduced pressure in order
  2. customto remove methanol
  3. extractionThe aqueous mixture is extracted with ethyl acetate
  4. washthe organic phase is washed with saturated aqueous sodium chloride solution
  5. customevaporated
  6. customFinally, the residue is recrystallized from methylene chloride/n-hexane

출처 및 근거

ORD 기록
ord-f4efa9d6aa6846789db741a00ed5ed54
출처 데이터셋
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04699652

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