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

HRID 358927

반응식

HRID 358927 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
95 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6fd7ed6bceeb475aa404fdac8da39a05
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04997987

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