反応式
C1(N)C([N+:7]([O-:9])=[O:8])=C(N)C([N+]([O-])=O)=C(N)C=1[N+]([O-])=O.[C:19]1([CH:27]=[C:25]([OH:26])[CH:24]=[C:22]([OH:23])[CH:21]=1)[OH:20].[N:28]([O-:30])=[O:29].[Na+].[N+:32]([O-])([OH:34])=[O:33]>>[N+:7]([C:27]1[C:19]([OH:20])=[C:21]([N+:28]([O-:30])=[O:29])[C:22]([OH:23])=[C:24]([N+:32]([O-:34])=[O:33])[C:25]=1[OH:26])([O-:9])=[O:8]参加物
実験手順
Another method of synthesizing TATB from phloroglucinol is described in GB 2355715. The phloroglucinol is nitrated using sodium nitrite and nitric acid, forming trinitrophloroglucinol (“TNPG”), which is also known as 1,3,5-trihydroxy-2,4,6-trinitrobenzene. The nitric acid is added sequentially or in multiple additions. When cooled, a solid is produced, which is filtered, washed with 3M hydrochloric acid (“HCl”), and dried, yielding a solid product that is a monohydrate of TNPG. The monohydrate of TNPG is a free-flowing solid. The TNPG is alkoxylated using a trialkyl orthoformate, such as triethyl orthoformate (“TEOF”), forming 1,3,5-triethoxy-2,4,6-trinitrobenzene (“TETNB”). The alkoxylation of TNPG requires a ninefold molar excess of triethyl orthoformate, producing a waste stream of ethyl formate, ethanol, and diethyl ether. The ethanol and ethyl formate are removed by distillation. The solution of TETNB is concentrated, yielding TETNB as a solid, which is recrystallized from ethanol. The purified TETNB is aminated using liquid ammonia, filtered, washed with N-methylpyrrolidinone and methanol, and dried, yielding crystals of the TATB. The TATB synthesis utilizes multiple drying and isolation acts to produce solid products of TNPG, TETNB, and TATB.
出典と根拠
- ORDレコード
- ord-6ae7368fdd3443b4a84e91c7c9a320ea
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07910776B2
関連ノート
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