Water → 5,5'-[Methylenebis(oxy)]bis(4,4-dinitropentan-1-ol)

HRID 255390노트

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HRID 255390 반응식
[N+:1]([C:4]([N+:29]([O-:31])=[O:30])([CH2:11][O:12][CH2:13][O:14][CH2:15][C:16]([N+:26]([O-:28])=[O:27])([N+:23]([O-:25])=[O:24])[CH2:17][CH2:18][C:19](OC)=[O:20])[CH2:5][CH2:6][C:7](OC)=[O:8])([O-:3])=[O:2].O>B.C1COCC1>[N+:1]([C:4]([N+:29]([O-:31])=[O:30])([CH2:11][O:12][CH2:13][O:14][CH2:15][C:16]([N+:23]([O-:25])=[O:24])([N+:26]([O-:28])=[O:27])[CH2:17][CH2:18][CH2:19][OH:20])[CH2:5][CH2:6][CH2:7][OH:8])([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 962Water2회HCID 20165452HCID 20165452, 화합물

생성물 1

HCID 230483335,5'-[Methylenebis(oxy)]bis(4,4-dinitropentan-1-ol)

시약·촉매·용매 1

HCID 2723981Borane;tetrahydrofuran용매

실험 절차

Dimethyl 4,4,10,10-tetranitro-6,8-dioxatridecane-1,13-dioate (28.8 g) was dissolved in 139 mL of BH3.THF with ice-cooling and under a nitrogen atmosphere. The solution was stirred at room temperature for 3 days, after which time 27 mL of water was added slowly and the mixture was heated at 60° C. for 5 minutes. After cooling, the mixture was poured into 200 mL of water, and the product was extracted with ether. The ether solution was washed with aqueous sodium bicarbonate solution, then with water, and dried (MgSO4) After removal of the solvent, the crude product was recrystallized from dichloromethane. Yield: 19.9 g (79%); M.P. 72.5°-3.5° C. 1H NMR spectrum (CDCl3 /TMS): δ 4.76 (s, 2H); 4.41 (s, 4H); 2.69 (m, 4H); 1.59 (m. 4H).

후처리

  1. temperaturecooling and under a nitrogen atmosphere
  2. temperaturethe mixture was heated at 60° C. for 5 minutes
  3. temperatureAfter cooling
  4. extractionthe product was extracted with ether
  5. washThe ether solution was washed with aqueous sodium bicarbonate solution
  6. dry with materialwith water, and dried (MgSO4)
  7. customAfter removal of the solvent
  8. customthe crude product was recrystallized from dichloromethane

출처 및 근거

ORD 기록
ord-43b4e8df805249e79b05612a754afddb
출처 데이터셋
uspto-grants-1987_10
특허 번호
USH0000351

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