Water → HCID 22643430、化合物

HRID 2414782ノート

反応式

HRID 2414782 の反応式
[SH:1][C:2]1[NH:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.Br[CH:12]([CH3:24])[CH2:13][CH2:14][C:15]([N:17]1[CH2:22][CH2:21][CH:20]([CH3:23])[CH2:19][CH2:18]1)=[O:16].C(N(CC)CC)C.O>C(#N)C>[N:3]1[C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[NH:6][C:2]=1[S:1][CH:12]([CH3:24])[CH2:13][CH2:14][C:15]([N:17]1[CH2:22][CH2:21][CH:20]([CH3:23])[CH2:19][CH2:18]1)=[O:16]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 226434181-(4-Bromovaleroyl)-4-methylpiperidineHCID 178527775HCID 178527775、化合物

生成物 1

HCID 22643430HCID 22643430、化合物収率 21.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

0.15 g of 2-mercaptobenzimidazole and 0.26 g of 1-(4-bromovaleroyl)-4-methylpiperidin were suspended in acetonitrile, and the suspension was added with 0.17 ml of triethylamine and refluxed for 7 hours. The reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with water and dried over sodium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (methanol:methylene chloride=1:10) to obtain 0.07 g of the title compound as oil (yield: 21%).

後処理

  1. temperaturerefluxed for 7 hours
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialdried over sodium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (methanol:methylene chloride=1:10)

出典と根拠

ORDレコード
ord-b91d2aeead8044b499cc2c21461ad4a6
出典データセット
uspto-grants-2004_11
特許番号
US06815455B1

反応ノート

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