Hydrochloric Acid → HCID 15341788、化合物

HRID 1033619ノート

反応式

HRID 1033619 の反応式
[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].[CH3:16][NH2:17].[Cl-].[NH4+].Cl>>[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]([NH:17][CH3:16])=[O:5]

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 6329MethylamineHCID 25517Ammonium ChlorideHCID 13019279Methyl 2,4-dihydroxy-3-(prop-2-en-1-yl)benzoate

生成物 1

HCID 15341788HCID 15341788、化合物収率 75%

実験手順

the compound of Example 5 (3.5 g) and excess methyl amine 40% aqueous solution) were stirred overnight at 50° C. in the presence of a few crystals of ammonium chloride. The reaction mixture was cooled and neutralized with 10% hydrochloric acid then extracted with ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated under vacuum. The crude crystals were dissolved in chloroform and then hexane was added until the product precipitated out of solution. The precipitate was filtered and dried to give the product (2.5 g, 75% yield).

後処理

  1. temperatureThe reaction mixture was cooled
  2. extractionthen extracted with ethyl acetate
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated under vacuum
  5. dissolutionThe crude crystals were dissolved in chloroform
  6. additionhexane was added until the product
  7. customprecipitated out of solution
  8. filtrationThe precipitate was filtered
  9. customdried

出典と根拠

ORDレコード
ord-9fa2d9393d3a465bb68d3dd456b1ab21
出典データセット
uspto-grants-1994_05
特許番号
US05310951

反応ノート

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