Triethylamine → METHYL 3-(HYDROXYMETHYL)-5-NITROBENZOATE

HRID 1531939

반응식

HRID 1531939 반응식
Cl[C:2]([C:4]1[CH:5]=[C:6]([CH:11]=[C:12]([N+:14]([O-:16])=[O:15])[CH:13]=1)[C:7]([O:9][CH3:10])=[O:8])=[O:3].[BH4-].[Na+].C(N(CC)CC)C>O1CCOCC1>[OH:3][CH2:2][C:4]1[CH:5]=[C:6]([CH:11]=[C:12]([N+:14]([O-:16])=[O:15])[CH:13]=1)[C:7]([O:9][CH3:10])=[O:8]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 74774Methyl 3-(chlorocarbonyl)-5-nitrobenzoateHCID 4311764Sodium borohydride

생성물 1

HCID 10703703METHYL 3-(HYDROXYMETHYL)-5-NITROBENZOATE

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A stirred solution of the product from step (i) (46.54 g) and sodium borohydride (13.01 g) in 1,4-dioxane (200 ml) was heated at reflux for 17 hours. The mixture was cooled and treated with triethylamine (27.9 ml), poured onto ice-water and extracted with ethyl acetate. The combined extracts were dried (MgSO4) and evaporated. The product was recrystallised from isohexane. Yield 19.38 g.

후처리

  1. temperatureat reflux for 17 hours
  2. temperatureThe mixture was cooled
  3. additionpoured onto ice-water
  4. extractionextracted with ethyl acetate
  5. dry with materialThe combined extracts were dried (MgSO4)
  6. customevaporated
  7. customThe product was recrystallised from isohexane

출처 및 근거

ORD 기록
ord-8ae2dc45fa73405cbbda1d2570d69ebf
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06200981B1

연결된 노트

불러오는 중…