Water → HCID 22643430, 화합물

HRID 2414782노트

반응식

HRID 2414782 반응식
[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]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 226434181-(4-Bromovaleroyl)-4-methylpiperidineHCID 178527775HCID 178527775, 화합물

생성물 1

HCID 22643430HCID 22643430, 화합물수율 21.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-b91d2aeead8044b499cc2c21461ad4a6
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06815455B1

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