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Water → 1-{1,4-Dioxaspiro[4.5]decan-8-yl}methanamine

HRID 2396738
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HRID 2396738 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[O:7]1[C:11]2([CH2:16][CH2:15][CH:14]([C:17]([NH2:19])=O)[CH2:13][CH2:12]2)[O:10][CH2:9][CH2:8]1.O.ClCCl>C1COCC1>[NH2:19][CH2:17][CH:14]1[CH2:15][CH2:16][C:11]2([O:7][CH2:8][CH2:9][O:10]2)[CH2:12][CH2:13]1
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참가 물질

6

반응물 4

HCID 962WaterHCID 6344DichloromethaneHCID 192616901,4-Dioxaspiro[4.5]decane-8-carboxamideHCID 21226445Aluminium lithium hydride

생성물 1

HCID 109539781-{1,4-Dioxaspiro[4.5]decan-8-yl}methanamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To 1.4 g (0.037 mole) of lithium aluminum hydride in 100 ml dry THF is added, portionwise, 4.9 g (0.026 mole) of 1,4-dioxaspiro[4,5]decane-8-carboxamide over one-half hour. This mixture is then refluxed 2 hours, then allowed to cool to room temperature. About 5 ml water is added cautiously and then stirred 15 minutes. Dichloromethane is then added and the insolubles filtered off. The organic layer is dried over MgSO4 and stripped to dryness, giving 3.48 g crude product. This material is vacuum-distilled to obtain 8-aminomethyl-1,4-dioxaspiro[4,5]decane (b.p. 84°-101° C. at 0.7 mm Hg.)

후처리

  1. temperatureThis mixture is then refluxed 2 hours
  2. filtrationthe insolubles filtered off
  3. dry with materialThe organic layer is dried over MgSO4
  4. customgiving 3.48 g crude product
  5. distillationThis material is vacuum-distilled

출처 및 근거

ORD 기록
ord-9360af0fbdac4df2ab78c9459014c2de
출처 데이터셋
uspto-grants-1996_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05494918

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