Ammonium Chloride → HCID 15341803, 화합물

HRID 893453노트

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HRID 893453 반응식
[OH:1][C:2]1[C:11]([CH2:12][CH:13]=[CH2:14])=[C:10]([OH:15])[CH:9]=[CH:8][C:3]=1[C:4](OC)=[O:5].[Cl-].[NH4+:17]>C(O)C>[OH:1][C:2]1[C:11]([CH2:12][CH:13]=[CH2:14])=[C:10]([OH:15])[CH:9]=[CH:8][C:3]=1[C:4]([NH2:17])=[O:5]

참가 물질

4

반응물 2

HCID 25517Ammonium ChlorideHCID 13019279Methyl 2,4-dihydroxy-3-(prop-2-en-1-yl)benzoate

생성물 1

HCID 15341803HCID 15341803, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
50 °C

실험 절차

Methyl 2,4-dihydroxy-3-(2-propenyl)benzoate (4.4 g) was added to a mixture of about 10 to 15 ml of saturated ammonium chloride solution and 2 to 3 ml of ethanol. The reaction mixture was stirred overnight at 50° C. The reaction mixture was extracted five times with ethyl acetate, and the organic layer was concentrated under vacuum. The product was crystallized and recrystallized from chloroform. Subsequent chromatography of the precipitated product on a 25 g silica gel column with 40% ethyl acetate/hexane as eluant gave the pure product.

후처리

  1. extractionThe reaction mixture was extracted five times with ethyl acetate
  2. concentrationthe organic layer was concentrated under vacuum
  3. customThe product was crystallized
  4. customrecrystallized from chloroform
  5. customSubsequent chromatography of the precipitated product on a 25 g silica gel column with 40% ethyl acetate/hexane as eluant gave the pure product

출처 및 근거

ORD 기록
ord-b34b2ae59d3848c7b2f3540be1d3827b
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05124350

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