Methanol → HCID 21556923, 화합물

HRID 267331

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HRID 267331 반응식
[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([N+:11]([O-:13])=[O:12])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15].Cl[C:18]1[C:19]([N+:45]([O-:47])=[O:46])=[C:20]([C:30]2[C:35]([N+:36]([O-:38])=[O:37])=[CH:34][C:33]([N+:39]([O-:41])=[O:40])=[CH:32][C:31]=2[N+:42]([O-:44])=[O:43])[C:21]([N+:27]([O-:29])=[O:28])=[CH:22][C:23]=1[N+:24]([O-:26])=[O:25].CO>CC(C)=O>[N+:8]([C:7]1[CH:6]=[C:5]([N+:11]([O-:13])=[O:12])[CH:4]=[C:3]([N+:14]([O-:16])=[O:15])[C:2]=1[CH2:1][C:22]1[C:21]([N+:27]([O-:29])=[O:28])=[C:20]([C:30]2[C:31]([N+:42]([O-:44])=[O:43])=[CH:32][C:33]([N+:39]([O-:41])=[O:40])=[CH:34][C:35]=2[N+:36]([O-:38])=[O:37])[C:19]([N+:45]([O-:47])=[O:46])=[CH:18][C:23]=1[N+:24]([O-:26])=[O:25])([O-:10])=[O:9]

참가 물질

5

반응물 3

HCID 887MethanolHCID 83762,4,6-TrinitrotolueneHCID 14927170HCID 14927170, 화합물

생성물 1

HCID 21556923HCID 21556923, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

The reaction of 4.5 g (0.02 mole) of TNT with 4.6 g, (0.01 mole) of 3-chloro-2,2',4,4',6,6'-hexanitrobiphenyl was carried out as above. After extracting the crude reaction product with methanol until the extracts were light colored, the somewhat gummy residue was dissolved in acetone, an equal volume of methanol was added and the solution was heated, with magnetic stirring, on a hot plate. A light yellow crystalline material separated, was filtered off and dried. It weighed 1.7 g, 25% of the theoretical yield. Recrystallized from acetone methanol formed faintly yellow rod-like crystals, mp 255°-256°. Anal. Calcd for C19H7N9O18 : C, 35.1; H, 1.1; N, 19.4. Found: C, 34.9, 34.2; H, 1.6, 1.2; N, 19.2, 18.8.

후처리

  1. extractionAfter extracting the crude
  2. customreaction product with methanol until the extracts
  3. temperaturethe solution was heated, with magnetic stirring, on a hot plate
  4. customA light yellow crystalline material separated
  5. filtrationwas filtered off
  6. customdried
  7. customRecrystallized from acetone methanol
  8. customformed faintly yellow rod-like crystals, mp 255°-256°

출처 및 근거

ORD 기록
ord-8d32c2f24e7b4d6f9293d7a817d07d8f
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03941853

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