Dibenzothiophene, 3,7-dinitro-, 5-oxide → Dibenzo[b,d]thiophene-3,7-diamine

HRID 79815ノート

反応式

HRID 79815 の反応式
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[C:11]3[CH:12]=[CH:13][C:14]([N+:16]([O-])=O)=[CH:15][C:10]=3[S:9](=O)[C:8]=2[CH:20]=1)([O-])=O>C(O)C.[Pd]>[CH:12]1[C:11]2[C:7]3[CH:6]=[CH:5][C:4]([NH2:1])=[CH:20][C:8]=3[S:9][C:10]=2[CH:15]=[C:14]([NH2:16])[CH:13]=1

参加物

4

反応物 1

HCID 15487214Dibenzothiophene, 3,7-dinitro-, 5-oxide

生成物 1

HCID 9990823Dibenzo[b,d]thiophene-3,7-diamine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

Two batches of the above solid 3,7-dinitro-dibenzothiophene 5-oxide was hydrogenated at 45 psi in ethanol (250 mL for each batch) with 10% Pd on carbon (0.46 g each batch) for 2 hours. Two batches were combined and filtered through CELITE to give an orange solution. Hydrogen chloride gas was bubbled into the solution to form precipitate (at pH 1). The precipitate was filtered and washed with small amount of ethanol and dried on vacuum to give an orange solid Dibenzothiophene-3,7-diamine (2.46 g). LCMS-ESI−: calc'd for C12H10N2S: 214.29. Found: 215.0 (M+H+).

後処理

  1. customfor 2 hours
  2. filtrationfiltered through CELITE
  3. customto give an orange solution
  4. customHydrogen chloride gas was bubbled into the solution to form precipitate (at pH 1)
  5. filtrationThe precipitate was filtered
  6. washwashed with small amount of ethanol
  7. customdried on vacuum

出典と根拠

ORDレコード
ord-a0a8a002d31240ed87639285a87a983d
出典データセット
uspto-grants-2014_09
特許番号
US08841278B2

反応ノート

読み込み中…