Isopropanol → HCID 19603840, 화합물

HRID 2292490노트

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HRID 2292490 반응식
[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([N+:19]([O-:21])=[O:20])=[C:13]([CH2:15][C:16]([OH:18])=[O:17])[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:22][CH:23](O)[CH3:24].Cl.C(N=C=NCCCN(C)C)C>C(Cl)Cl.CN(C)C1C=CN=CC=1>[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([N+:19]([O-:21])=[O:20])=[C:13]([CH2:15][C:16]([O:18][CH:23]([CH3:24])[CH3:22])=[O:17])[CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 3

HCID 3776IsopropanolHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 19603791HCID 19603791, 화합물

생성물 1

HCID 19603840HCID 19603840, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

To a solution of 5-benzyloxy-2-nitrophenylacetic acid (25.1 g) in methylene chloride (250 ml) were added in turn 2-propanol (27 ml), 4-dimethylaminopyridine (1.07 and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (18.4 g) and the resulting mixture was stirred at room temperature for one hour and then allowed to stand overnight. After the solvent was distilled off under reduced pressure, the resulting residue was diluted with ethyl acetate, washed subsequently with 1N hydrochloric acid and saturated saline. The organic layer was dried over magnesium sulfate and distilled off under reduced pressure. The dark yellow oily substance thus obtained (29.7 g) was purified by a silica gel column chromatography (hexane:ethyl acetate=4:1) to give the title compound (22.5 g).

후처리

  1. waitto stand overnight
  2. distillationAfter the solvent was distilled off under reduced pressure
  3. additionthe resulting residue was diluted with ethyl acetate
  4. washwashed subsequently with 1N hydrochloric acid and saturated saline
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. distillationdistilled off under reduced pressure
  7. customThe dark yellow oily substance thus obtained (29.7 g)
  8. customwas purified by a silica gel column chromatography (hexane:ethyl acetate=4:1)

출처 및 근거

ORD 기록
ord-2e53e0f9c9804bdea1c91b5f03f68570
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05684003

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