Water → HCID 19976898, 화합물

HRID 1450641노트

반응식

HRID 1450641 반응식
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([NH:9]Cl)=O)=[CH:5][CH:4]=1.[CH:13]#[C:14][CH:15]([OH:18])[CH2:16][CH3:17].C(N(CC)CC)C.[OH2:26]>C1C=CC=CC=1>[OH:18][CH:15]([C:16]1[O:26][N:9]=[C:7]([C:6]2[CH:11]=[CH:12][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[CH:17]=1)[CH2:14][CH3:13]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 929811-Pentyn-3-olHCID 21579386N-Chloro-4-methoxybenzamide

생성물 1

HCID 19976898HCID 19976898, 화합물

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

To a solution of 79.8 g (43 mmol) of 4-methoxybenzhydroxamic acid chloride and 7.23 g (86 mmol) of 1-pentyn-3-ol in 160 ml of benzene, a solution of 6.53 g (64.5 mmol) of triethylamine in 80 ml of benzene was added dropwise while maintaining the internal temperature at 3°-5° C. After the mixture was stirred for 2 hours, water was added so that the reaction product was extracted in the organic layer. The organic layer was separated and collected and the solvent was distilled off, whereby an oily residue was obtained. The oily residue was purified by silica gel chromatography (eluent: 30:1 chloroform/methyl alcohol), so that the title compound was obtained as yellow oil [yield: 8.07 g (81%)].

후처리

  1. temperaturewhile maintaining the internal temperature at 3°-5° C
  2. extractionwas extracted in the organic layer
  3. customThe organic layer was separated
  4. customcollected
  5. distillationthe solvent was distilled off
  6. customwhereby an oily residue was obtained
  7. customThe oily residue was purified by silica gel chromatography (eluent: 30:1 chloroform/methyl alcohol), so that the title compound
  8. customwas obtained as yellow oil [yield: 8.07 g (81%)]

출처 및 근거

ORD 기록
ord-851347d028ff47a1b3d7f54c890645d2
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05602160

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