Water → 2-(1,4-Dioxaspiro(4.5)decan-8-yl)ethan-1-ol

HRID 500088

반응식

HRID 500088 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[O:7]1[C:11]2([CH2:16][CH2:15][CH:14]([CH2:17][C:18](OCC)=[O:19])[CH2:13][CH2:12]2)[O:10][CH2:9][CH2:8]1.[F-].[Na+].O>O1CCCC1.ClCCl>[OH:19][CH2:18][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

참가 물질

7

반응물 4

HCID 962WaterHCID 5235Sodium FluorideHCID 15700391Ethyl 2-(1,4-dioxaspiro[4.5]decan-8-yl)acetateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 118054582-(1,4-Dioxaspiro(4.5)decan-8-yl)ethan-1-ol수율 102.5%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
25 °C

실험 절차

To a mixture of lithium aluminium hydride (831 mg) and anhydrous tetrahydrofuran (70 ml) at 0° C. was added a solution of ethyl 1,4-dioxaspiro[4.5]decane-8-acetate of Example 90 (2) (5.0 g) in anhydrous tetrahydrofuran (30 ml). The mixture was gradually warmed to about 25° C., stirred for 3 hours, and then sodium fluoride, water and dichloromethane were added to the reaction mixture. The precipitate was filtrated off with Celite, the filtrated organic layer was dried over sodium sulfate. The solvent was removed in vacuo from the organic layer to give 4.18 g of 8-(2-hydroxyethyl)-1,4-dioxaspiro[4.5]decane.

후처리

  1. filtrationThe precipitate was filtrated off with Celite
  2. dry with materialthe filtrated organic layer was dried over sodium sulfate
  3. customThe solvent was removed in vacuo from the organic layer

출처 및 근거

ORD 기록
ord-ebc26539d1f845a08a41f540767d9e96
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07767854B2

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