Glutaric anhydride → Pentaerythritol trinitrate glutarate

HRID 2380393

반응식

HRID 2380393 반응식
[N+:1]([O:4][CH2:5][C:6]([CH2:17][OH:18])([CH2:12][O:13][N+]([O-])=O)[CH2:7][O:8][N+]([O-])=O)([O-:3])=[O:2].[C:19]1(=[O:26])[O:25][C:23](=[O:24])[CH2:22][CH2:21][CH2:20]1>CN(C)C1C=CN=CC=1.CCOCC>[C:19]([OH:25])(=[O:26])[CH2:20][CH2:21][CH2:22][C:23]([OH:2])=[O:24].[N+:1]([O-:4])([OH:3])=[O:2].[N+:1]([O-:4])([OH:3])=[O:2].[N+:1]([O-:4])([OH:3])=[O:2].[OH:4][CH2:5][C:6]([CH2:17][OH:18])([CH2:12][OH:13])[CH2:7][OH:8]

참가 물질

5

반응물 2

HCID 7940Glutaric anhydrideHCID 15353Pentaerythritol, trinitrate

생성물 1

HCID 86748279Pentaerythritol trinitrate glutarate수율 145.8%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 3283Diethyl Ether용매

실험 절차

Pentaerythritol trinitrate (0.8 gram, 0.003 mol) was combined with 0.4 gram (0.03 mol) of glutaric anhydride and 50 mg of 4-dimethylamino pyridine in 25 ml of ether. The mixture was stirred at boiling for 12 hours and concentrated under vacuum, then the oily residue was partitioned between ether and saturated NaHCO3. The aqueous base layer was removed and acidified with 1N HCl to approximately pH 6. The solution was cooled in ice and after 15 minutes a white precipitate was collected, washed with water and air dried, yielding 0.5 gram of pentaerythritol trinitrate glutarate in the form of a white powder.

후처리

  1. concentrationconcentrated under vacuum
  2. customthe oily residue was partitioned between ether and saturated NaHCO3
  3. customThe aqueous base layer was removed
  4. temperatureThe solution was cooled in ice and after 15 minutes a white precipitate
  5. customwas collected
  6. washwashed with water and air
  7. customdried

출처 및 근거

ORD 기록
ord-cef31c830bfe4aa68ae78394ae15c614
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05367061

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