Tetrahydrofuran → HCID 86662689, 화합물

HRID 1746335노트

반응식

HRID 1746335 반응식
[C:1]1([CH2:17][CH2:18][CH2:19][CH2:20]O)[C:14]2[C:15]3=[C:16]4[C:11](=[CH:12][CH:13]=2)[CH:10]=[CH:9][CH:8]=[C:7]4[CH:6]=[CH:5][C:4]3=[CH:3][CH:2]=1.C(N(CC)CC)C.[C:29](Cl)(=[O:33])[C:30]([CH3:32])=[CH2:31].[O:35]1CCCC1>>[C:29]([O:33][CH:17]([C:1]1[C:14]2[C:15]3=[C:16]4[C:11](=[CH:12][CH:13]=2)[CH:10]=[CH:9][CH:8]=[C:7]4[CH:6]=[CH:5][C:4]3=[CH:3][CH:2]=1)[CH2:18][CH2:19][CH3:20])(=[O:35])[C:30]([CH3:32])=[CH2:31]

참가 물질

5

반응물 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 13528Methacryloyl chlorideHCID 27626721-Pyrenebutanol

생성물 1

HCID 86662689HCID 86662689, 화합물

실험 절차

In 100 ml of tetrahydrofuran, 5.0 g of 1-pyrenebutanol and 3.68 g of triethylamine were dissolved, and 1.90 g of methacryloyl chloride was added dropwise thereto at 0° C., followed by stirring at room temperature for 1 hour. A deposited material was filtered while being washed with ethyl acetate. The filtrate and the washing liquid were mixed. After the mixture was dried with magnesium sulfate, the solvent was removed by evaporation under a reduced pressure. A residue was purified by a column chromatograph (silica gel, hexane:ethyl acetate=10:1), and vacuum-dried to thus obtain 1-pyrenylbutyl methacrylate.

후처리

  1. customat 0° C.
  2. filtrationA deposited material was filtered
  3. washwhile being washed with ethyl acetate
  4. additionThe filtrate and the washing liquid were mixed
  5. dry with materialAfter the mixture was dried with magnesium sulfate
  6. customthe solvent was removed by evaporation under a reduced pressure
  7. customA residue was purified by a column chromatograph (silica gel, hexane:ethyl acetate=10:1)
  8. dry with materialvacuum-dried to thus obtain 1-pyrenylbutyl methacrylate

출처 및 근거

ORD 기록
ord-7416e88d2e8b466a9a4890b54f645be9
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09150414B2

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