Hydroquinone → HCID 66968668, 화합물

HRID 1522693노트

반응식

HRID 1522693 반응식
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][C:8]1[CH:20]=[CH:19][C:11]([O:12]C2CCCCO2)=[CH:10][CH:9]=1.[O:21]1[CH:26]=[CH:25][CH2:24][CH2:23][CH2:22]1.C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1.C1(C=CC(O)=CC=1)O>C(Cl)Cl>[C:8]1([CH:20]=[CH:19][C:11]([OH:12])=[CH:10][CH:9]=1)[OH:7].[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[O:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1

참가 물질

6

반응물 4

HCID 785HydroquinoneHCID 80803,4-dihydro-2H-pyranHCID 2973612,2'-[1,4-Phenylenebis(oxy)]bis(oxane)HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)

생성물 1

HCID 66968668HCID 66968668, 화합물수율 75%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Another functionalization substance may be 2-[2-(undec-10-enyl)-4-(tetrahydro-2H-pyran-2-yloxy) phenoxy]tetrahydro-H-pyran. This molecule, whose structure is shown in FIG. 13, may be synthesized from 2-[4-(tetrahydro-2H-pyran-2-yloxy) phenoxy]tetrahydro-2H-pyran using any prior art process. The intermediate may be synthesized by first adding dihydropyran (0.83 mL, 9.1 mmol) and pyridinium p-toluenesulfonate (0.11 g, 0.45 mmol) to a solution of hydroquinone (0.25 g, 2.3 mmol) in CH2Cl2 (3 mL). This reaction mixture is then stirred for about 12 hours and diluted with 10 mL of CH2Cl2. The mixture is subsequently washed by 3×5 mL of NaHCO3 and 1×5 mL brine, dried over MgSO4, and concentrated to a white solid. Silica gel chromatography (4:1 hexane/ethyl acetate) provides the di-tetrahydropyran hydroquinone as a white solid (0.48 mg, 75%).

후처리

  1. customThe intermediate may be synthesized
  2. washThe mixture is subsequently washed by 3×5 mL of NaHCO3 and 1×5 mL brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated to a white solid

출처 및 근거

ORD 기록
ord-a2cae41a7d3d42e79a826811d3697528
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09076665B2

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