Trimesoyl chloride → HCID 58979968、化合物

HRID 1180687

反応式

HRID 1180687 の反応式
N1[C:5]([C:6]2[CH:19]=[CH:18][C:17]3[C:8](=[C:9]4[C:14](=[CH:15][CH:16]=3)[CH:13]=[CH:12][CH:11]=[N:10]4)[N:7]=2)=[N:4][N:3]=N1.[C:20]1([C:32](Cl)=[O:33])[CH:25]=[C:24]([C:26](Cl)=[O:27])[CH:23]=[C:22]([C:29](Cl)=[O:30])[CH:21]=1>N1C=CC=CC=1>[N:7]1[C:8]2[C:17](=[CH:16][CH:15]=[C:14]3[C:9]=2[N:10]=[CH:11][CH:12]=[CH:13]3)[CH:18]=[CH:19][C:6]=1[C:5]1[O:33][C:32]([C:20]2[CH:25]=[C:24]([C:26]3[O:27][C:5]([C:6]4[CH:19]=[CH:18][C:17]5[C:8](=[C:9]6[C:14](=[CH:15][CH:16]=5)[CH:13]=[CH:12][CH:11]=[N:10]6)[N:7]=4)=[N:4][N:3]=3)[CH:23]=[C:22]([C:29]3[O:30][C:5]([C:6]4[CH:19]=[CH:18][C:17]5[C:8](=[C:9]6[C:14](=[CH:15][CH:16]=5)[CH:13]=[CH:12][CH:11]=[N:10]6)[N:7]=4)=[N:4][N:3]=3)[CH:21]=2)=[N:3][N:4]=1

参加物

4

反応物 2

HCID 78138Trimesoyl chlorideHCID 178420729HCID 178420729、化合物

生成物 1

HCID 58979968HCID 58979968、化合物収率 44.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
85 °C

実験手順

To a flask was added a mixture of 15 g 2-(1H-tetrazol-5-yl)-[1,10]phenanthroline and 300 ml pyridine. The mixture was then heated to 80-90° C., and 4.86 g 1,3,5 benzene tricarbonyl chloride was added. Subsequently, the mixture solution was heated to 110° C. and stirred overnight. After completion of reaction, as shown in scheme 8, the reaction mixture was filtered to collect solids. The solids was washed by pyridine and CH2Cl2 respectively, and then dried on oven to obtain products 6.6 g (yield=44.1%). MS(m/z, FAB+), 888, 810, 521, 444, 155.

後処理

  1. additionTo a flask was added
  2. temperatureSubsequently, the mixture solution was heated to 110° C.
  3. customAfter completion of reaction
  4. filtrationthe reaction mixture was filtered
  5. customto collect solids
  6. washThe solids was washed by pyridine and CH2Cl2 respectively
  7. customdried on oven

出典と根拠

ORDレコード
ord-42c58dc405e44091894b97aeb08b019a
出典データセット
uspto-grants-2007_10
特許番号
US07282586B1

関連ノート

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