Hydrochloric Acid → HCID 21882727、化合物

HRID 722048ノート

反応式

HRID 722048 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][N:6]=[C:5]([CH2:9][CH2:10][C:11]([O:13]C)=[O:12])[CH:4]=1.[OH-].[Na+].Cl>O1CCCC1>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][N:6]=[C:5]([CH2:9][CH2:10][C:11]([OH:13])=[O:12])[CH:4]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21882722Methyl 3-(4-methoxypyridin-2-yl)propanoate2 回

生成物 1

HCID 21882727HCID 21882727、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

41.95 g of methyl 3-(4-methoxypyridin-2-yl)propionate (starting material A2) are dissolved in 700 ml of tetrahydrofuran, and 217 ml of 1N sodium hydroxide solution are added. The mixture is stirred at room temperature until no more starting material is detectable by thin-layer chromatography (TLC). The mixture is neutralized using 217 ml of 1N hydrochloric acid solution, evaporated to dryness using a rotary evaporator and dried under high vacuum. The colorless residue is ground and extracted four times with dichloromethane/methanol (9:1). The combined extracts are evaporated to dryness. This gives 33.2 g of the title compound as a colorless powder of m.p. 131–132° C. The mass spectrum shows the molecular peak MH+ at 182 Da.

後処理

  1. customevaporated to dryness
  2. customa rotary evaporator
  3. customdried under high vacuum
  4. extractionextracted four times with dichloromethane/methanol (9:1)
  5. customThe combined extracts are evaporated to dryness

出典と根拠

ORDレコード
ord-8f81c94161ae4fa6b9a98235e9fee118
出典データセット
uspto-grants-2006_11
特許番号
US07138399B2

反応ノート

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