Sodium Hydroxide → 4-(1,4-Dioxaspiro[4.5]dec-7-en-8-yl)pyridine

HRID 980906노트

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HRID 980906 반응식
[CH2:1]1[O:17][C:4]2([CH2:9][CH2:8][C:7](O)([C:10]3[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=3)[CH2:6][CH2:5]2)[O:3][CH2:2]1.S(Cl)(Cl)=O.[OH-].[Na+]>N1C=CC=CC=1>[CH2:2]1[O:3][C:4]2([CH2:9][CH2:8][C:7]([C:10]3[CH:11]=[CH:12][N:13]=[CH:14][CH:15]=3)=[CH:6][CH2:5]2)[O:17][CH2:1]1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24386Thionyl ChlorideHCID 137720538-(4-Pyridinyl)-1,4-dioxaspiro[4.5]decan-8-ol

생성물 1

HCID 137720544-(1,4-Dioxaspiro[4.5]dec-7-en-8-yl)pyridine수율 86.6%

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
0 °C

실험 절차

To 5 g of 4-hydroxy-4-(4-pyridyl)cyclohexanone ethyleneacetal dissolved in 40 ml of pyridine, there was added 8 ml of thionyl chloride at -10° C. After stirring the mixture at 0° C., the reaction mixture was poured into ice water. Then, an excess amount of aqueous sodium hydroxide solution was added. The reaction mixture was extracted with methylene chloride and purified. Thus, there was obtained 4 g of 4-(4-pyridyl)cyclohex-3-enone ethyleneacetal.

후처리

  1. extractionThe reaction mixture was extracted with methylene chloride
  2. custompurified

출처 및 근거

ORD 기록
ord-6135d322c9364c05a30f77440b5214e6
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04639521

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