N-bromobutanimide → HCID 19977128、化合物

HRID 1450504ノート

反応式

HRID 1450504 の反応式
[CH3:1][C:2]1[C:3]2[CH:10]=[C:9]([C:11]3[N:12]=[N:13][N:14]([CH3:16])[N:15]=3)[CH:8]=[CH:7][C:4]=2[S:5][CH:6]=1.[Br:17]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Br:17][CH2:1][C:2]1[C:3]2[CH:10]=[C:9]([C:11]3[N:12]=[N:13][N:14]([CH3:16])[N:15]=3)[CH:8]=[CH:7][C:4]=2[S:5][CH:6]=1

参加物

5

反応物 2

HCID 67184N-bromobutanimideHCID 19977136HCID 19977136、化合物

生成物 1

HCID 19977128HCID 19977128、化合物収率 74.1%

試薬・触媒・溶媒 2

HCID 7187Benzoyl Peroxide触媒HCID 5943Carbon Tetrachloride溶媒

実験手順

To a refluxing mixture of 3-methyl-5-(2-methyltetrazol-5-yl) benzo[b]thiophene (0.162 g, 0.703 mmol) and benzoyl peroxide (10.6 mg) in carbon tetrachloride (10 ml) irradiated with two desk lamps (2×60W) was added N-bromosuccinimide (0.126 g, 0.707 mmol) in small portions. After the addition was complete the mixture was heated at reflux for a further 90 min, then filtered and the filtrate was evaporated in vacuo to leave an oil/solid mixture. Chromatography on flash silica, eluting with dichloromethane gave 0.161 g of crude 3-bromomethyl-5-(2-methyltetrazol-5-yl) benzo[b]thiophene as a colourless oil.

後処理

  1. additionAfter the addition
  2. temperaturewas heated
  3. temperatureat reflux for a further 90 min
  4. filtrationfiltered
  5. customthe filtrate was evaporated in vacuo
  6. customto leave an oil/solid mixture
  7. washChromatography on flash silica, eluting with dichloromethane

出典と根拠

ORDレコード
ord-0eb026a3f2f64325a1c9c9281802255b
出典データセット
uspto-grants-1997_02
特許番号
US05602163

反応ノート

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