Sodium Carbonate → {8-Fluoro-1,4-dioxaspiro[4.5]decan-8-yl}methanol

HRID 1043233노트

반응식

HRID 1043233 반응식
[FH:1].N1C=CC=CC=1.O1[C:10]2([CH2:19][CH2:18][CH2:17][CH2:16][C:13]3([O:15][CH2:14]3)[O:12][CH2:11]2)C1.[C:20]([O-:23])([O-])=O.[Na+].[Na+]>ClCCl>[F:1][C:18]1([CH2:20][OH:23])[CH2:17][CH2:16][C:13]2([O:12][CH2:11][CH2:14][O:15]2)[CH2:10][CH2:19]1

참가 물질

6

반응물 4

HCID 10340Sodium CarbonateHCID 64774Pyridine, hydrofluoride (1:1)HCID 86647914HCID 86647914, 화합물HCID 178435160HCID 178435160, 화합물

생성물 1

HCID 67225989{8-Fluoro-1,4-dioxaspiro[4.5]decan-8-yl}methanol

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of pyridine hydrofluoride (4 g) in dichloromethane (10 mL) was added dropwise to a solution of EXAMPLE 443A (1.7 g) in dichloromethane (20 mL) in a polyethylene bottle at 0° C. The mixture was stirred at room temperature overnight. The mixture was carefully poured over a mixture of ice-water and Na2CO3 and extracted with ethyl acetate (2×300 mL). After washing with water and brine, the organic layer was dried over Na2SO4, and filtered. Concentration of the filtrate gave the crude product.

후처리

  1. extractionextracted with ethyl acetate (2×300 mL)
  2. washAfter washing with water and brine
  3. dry with materialthe organic layer was dried over Na2SO4
  4. filtrationfiltered

출처 및 근거

ORD 기록
ord-816022b831694ddcb7d88497577ac72f
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08557983B2

반응 노트

불러오는 중…