Hydrochloric Acid → 4-(3,4-Dihydroxy-5-nitrophenyl)-3-methylbut-3-en-2-ol

HRID 1195941노트

반응식

HRID 1195941 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:12]=[C:13]([CH3:17])[C:14](=[O:16])[CH3:15])[CH:5]=[C:6]([N+:9]([O-:11])=[O:10])[C:7]=1[OH:8].[BH4-].[Na+].O.Cl>[OH-].[Na+]>[OH:1][C:2]1[CH:3]=[C:4]([CH:12]=[C:13]([CH3:17])[CH:14]([OH:16])[CH3:15])[CH:5]=[C:6]([N+:9]([O-:11])=[O:10])[C:7]=1[OH:8]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 4311764Sodium borohydrideHCID 540099494-(3,4-Dihydroxy-5-nitrophenyl)-3-methylbut-3-en-2-one

생성물 1

HCID 544528424-(3,4-Dihydroxy-5-nitrophenyl)-3-methylbut-3-en-2-ol

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

1.8 g of the product obtained in Example 6 was dissolved in 20 ml of 1N NaOH-solution and 4.0 g of sodium borohydride in small amount of water was added. The mixture was stirred over night at room temperature, acidified with hydrochloric acid and extracted with ether. The solvent was evaporated in vacuo and the residue purified in a silica gel column by using toluene-acetic acid dioxane (18:1:1). The product was crystallized from dichloromethane petroleum ether. Yield 0.80 g (44%), m.p. 102°-104° C.

후처리

  1. extractionextracted with ether
  2. customThe solvent was evaporated in vacuo
  3. customthe residue purified in a silica gel column
  4. customThe product was crystallized from dichloromethane petroleum ether

출처 및 근거

ORD 기록
ord-7cc3eccc59404964873c6d876bdaf098
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05112861

반응 노트

불러오는 중…