Dimethylformamide → 1,3,5-Trichloro-2,4,6-trinitrobenzene

HRID 358927

反応式

HRID 358927 の反応式
S(Cl)([Cl:3])=O.CN(C)C=O.[Cl:10][C:11]1[C:12]([N+:26]([O-:28])=[O:27])=[C:13](OC)[C:14]([N+:21]([O-:23])=[O:22])=[C:15]([Cl:20])[C:16]=1[N+:17]([O-:19])=[O:18]>C1(C)C=CC=CC=1>[Cl:10][C:11]1[C:12]([N+:26]([O-:28])=[O:27])=[C:13]([Cl:3])[C:14]([N+:21]([O-:23])=[O:22])=[C:15]([Cl:20])[C:16]=1[N+:17]([O-:19])=[O:18]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 147940571,3-Dichloro-5-methoxy-2,4,6-trinitrobenzene

生成物 1

HCID 175181,3,5-Trichloro-2,4,6-trinitrobenzene収率 95%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
95 °C

実験手順

Thionyl chloride (0.20 ml, 0.027 mol) and dimethylformamide (0.15 ml, 0.022 mol) were added to a solution of 5 (0.624 g, 0.020 mol) in toluene (2 ml) at 50° C. The mixture was stirred and heated to 95° C. over a period of 15 min. and maintained at that temperature for another hour. The pale yellow solution was washed with water, dried over magnesium sulfate, treated with activated carbon, filtered, and evaporated to give a cream-colored solid (0.600 g, 95% yield). The melting point of the material so obtained was 194-195° C. (195-196° C. after recrystallization from acetic acid).

後処理

  1. temperaturemaintained at that temperature for another hour
  2. washThe pale yellow solution was washed with water
  3. dry with materialdried over magnesium sulfate
  4. additiontreated with activated carbon
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-6fd7ed6bceeb475aa404fdac8da39a05
出典データセット
uspto-grants-1991_03
特許番号
US04997987

関連ノート

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