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Sodium Azide → 4'-(azidomethyl)-2,2-dimethyl-3,4-dihydro-2H,5H-spiro[benzo[h]chromene-6,2'-[1,3]dioxolan]-5-one

HRID 1159438
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HRID 1159438 반응식
CS(O[CH2:6][CH:7]1[CH2:11][O:10][C:9]2([C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[C:18]3[O:17][C:16]([CH3:26])([CH3:25])[CH2:15][CH2:14][C:13]=3[C:12]2=[O:27])[O:8]1)(=O)=O.[N-:28]=[N+:29]=[N-:30].[Na+]>CN(C=O)C.C(Cl)Cl>[N:28]([CH2:6][CH:7]1[CH2:11][O:10][C:9]2([C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[C:18]3[O:17][C:16]([CH3:26])([CH3:25])[CH2:15][CH2:14][C:13]=3[C:12]2=[O:27])[O:8]1)=[N+:29]=[N-:30]
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참가 물질

5

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HCID 33557Sodium AzideHCID 59514394(2,2-dimethyl-5-oxo-3,4-dihydro-2H,5H-spiro[benzo[h]chromene-6,2'-[1,3]dioxolan]-4'-yl)methyl methanesulfonate

생성물 1

HCID 595143904'-(azidomethyl)-2,2-dimethyl-3,4-dihydro-2H,5H-spiro[benzo[h]chromene-6,2'-[1,3]dioxolan]-5-one수율 15%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매
HCID 6344
Dichloromethane
용매

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온도
100 °C

실험 절차

To a solution of 4′-(hydroxymethyl)-2,2-dimethyl-3,4-dihydro-2H,5H-spiro[benzo[h]chromene-6,2′-[1,3]dioxolan]-5-one (316 mg, 1.0 mmol) in dichloromethane (2 mL) is added methanesulfonyl chloride (0.095 mL, 1.3 mmol) and triethylamine (0.163 mL, 1.24 mmol). The mixture is stirred at room temperature for 2 hours. The reaction mixture is washed with water (2×1.0 mL), dried over sodium sulfate and concentrated to provide (2,2-dimethyl-5-oxo-3,4-dihydro-2H,5H-spiro[benzo[h]chromene-6,2′-[1,3]dioxolan]-4′-yl)methyl methanesulfonate as a white solid (99% by LC/MS, UV 254 nm). The (2,2-dimethyl-5-oxo-3,4-dihydro-2H,5H-spiro[benzo[h]chromene-6,2′-[1,3]dioxolan]-4′-yl)methyl methanesulfonate (197 mg, 0.5 mmol) is dissolved in DMF (2 mL) followed by the addition of sodium azide (97 mg, 1.5 mmol). The reaction is heated at 80° C. for 24 hour and 100° C. for 12 h. The mixture is diluted with CH2Cl2 (4 mL), washed with water (2 ml) and concentrated. The organic layer is dried with sodium sulfate, concentrated under reduced pressure and purified by flash column chromatography (SiO2, 30% EtOAc in hexane) to provide 4′-(azidomethyl)-2,2-dimethyl-3,4-dihydro-2H,5H-spiro[benzo[h]chromene-6,2′-[1,3]dioxolan]-5-one (25 mg, 15%) as a white solid. 400 MHz 1H NMR (CDCl3) δ: 7.78-7.56 (m, 1H), 7.60-7.57 (m, 1H), 7.44-7.40 (m, 2H), 4.68-4.62 (m, 1H), 4.46-4.42 (m, 1H), 4.23 (t, J=8 Hz, 1H). 3.96-3.91 (m, 1H), 3.54-3.49 (m, 1H), 2.48-2.42 (m, 2H), 1.79 (t, J=6.8 Hz, 2H), 1.42 (d, J=3.2 Hz, 6H); LCMS: 342 [M+H].

후처리

  1. washwashed with water (2 ml)
  2. concentrationconcentrated
  3. dry with materialThe organic layer is dried with sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. custompurified by flash column chromatography (SiO2, 30% EtOAc in hexane)

출처 및 근거

ORD 기록
ord-b4b028f6b9554148ac76110e1cb90686
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07812051B2

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