Dimethylformamide → HCID 22503528, 화합물

HRID 1814437노트

반응식

HRID 1814437 반응식
[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]#[CH:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[C:16]1[CH:23]=[CH:22][CH:21]=[CH:20][C:17]=1[CH:18]=[O:19].C(N(CC)CC)C.CN(C)[CH:33]=[O:34]>>[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]#[C:14][C:16]1[CH:23]=[CH:22][C:21]([O:34][CH3:33])=[CH:20][C:17]=1[CH:18]=[O:19])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 811292-BromobenzaldehydeHCID 563182Hex-5-ynyloxymethyl-benzene

생성물 1

HCID 22503528HCID 22503528, 화합물

실험 절차

6-Benzyloxy-1-hexyne (5.60 g) and 2-bromo-benzaldehyde (2.90 g) were reacted in dimethylformamide (30 ml), in the presence of dichloro-bis-triphenylphosphinepalladium (0.40 g), cuprous iodide (0.20 g) and triethylamine (2.5 ml) in nitrogen atmosphere at 50° C. for 6 hr. The resulting reaction solution was evaporated, and ethyl acetate and water were added to the resulting residue. The resulting organic layer was washed with water and brine, and dried over magnesium sulfate. The solvent was evaporated, and the resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane system), to give 2.60 g of the title compound as a pale yellow oil. (1-2) 3-(4-Benzyloxybutyl)isoquinoline-2-oxide

후처리

  1. customThe resulting reaction solution
  2. customwas evaporated
  3. additionethyl acetate and water were added to the resulting residue
  4. washThe resulting organic layer was washed with water and brine
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was evaporated
  7. customthe resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane system)

출처 및 근거

ORD 기록
ord-cc4e552b0ffc4234840b7ec2488d436e
출처 데이터셋
uspto-grants-2005_04
특허 번호
US06875761B2

반응 노트

불러오는 중…