Hydrochloric Acid → HCID 21882727, 화합물

HRID 722048노트

반응식

HRID 722048 반응식
[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

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21882722Methyl 3-(4-methoxypyridin-2-yl)propanoate2회

생성물 1

HCID 21882727HCID 21882727, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8f81c94161ae4fa6b9a98235e9fee118
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07138399B2

반응 노트

불러오는 중…