4-Bromo-1,2-difluorobenzene → 8-(3,4-Difluorophenyl)-1,4-dioxaspiro[4.5]decan-8-ol

HRID 1858935노트

반응식

HRID 1858935 반응식
[CH2:1]1[O:11][C:4]2([CH2:9][CH2:8][C:7](=[O:10])[CH2:6][CH2:5]2)[O:3][CH2:2]1.Br[C:13]1[CH:18]=[CH:17][C:16]([F:19])=[C:15]([F:20])[CH:14]=1.[Mg]>C1COCC1>[F:19][C:16]1[CH:17]=[C:18]([C:7]2([OH:10])[CH2:6][CH2:5][C:4]3([O:3][CH2:2][CH2:1][O:11]3)[CH2:9][CH2:8]2)[CH:13]=[CH:14][C:15]=1[F:20]

참가 물질

5

반응물 3

HCID 676754-Bromo-1,2-difluorobenzeneHCID 5674151,4-Dioxaspiro[4.5]decan-8-oneHCID 5462224Magnesium

생성물 1

HCID 221221048-(3,4-Difluorophenyl)-1,4-dioxaspiro[4.5]decan-8-ol수율 38%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 1,4-cyclohexanedione monoethylene ketal (15.6 g, 100 mmole) in dry THF (250 ml) was reacted with a solution of the Grignard reagent prepared from 1-bromo-3,4-difluorobenzene (19 g, 100 mmole) and magnesium (2.4 g, 100 mmole) in dry THF at -60° C. as described in example 3 to give the product (38%, mp: 118-120° C.). Calc'd for C14H16F2O3 : C, 62.22%; H,5.97%. Found: C, 61.97%; H, 6.35%.

출처 및 근거

ORD 기록
ord-60ee75590285465f8fdef730df139d73
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06153611

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