Methanol → HCID 21556923、化合物

HRID 267331

反応式

HRID 267331 の反応式
[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]

参加物

5

反応物 3

HCID 887MethanolHCID 83762,4,6-TrinitrotolueneHCID 14927170HCID 14927170、化合物

生成物 1

HCID 21556923HCID 21556923、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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°

出典と根拠

ORDレコード
ord-8d32c2f24e7b4d6f9293d7a817d07d8f
出典データセット
uspto-grants-1976_03
特許番号
US03941853

関連ノート

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