돌아가기
Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 1643346생성일: 2026년 10월 27일

1,1,3,3-Tetramethylguanidine → (3E)-3-[[3,5-dimethyl-4-(phenylmethoxy)phenyl]methylene]-1,4-dioxaspiro[4.5]decan-2-one

https://huagongshe.com/reaction/1643346

반응식

참여 물질

역할이름HCID투입량
반응물1,1,3,3-TetramethylguanidineHCID 66460—
반응물Lithium ChlorideHCID 433294—
반응물4-(Benzyloxy)-3,5-dimethylbenzaldehydeHCID 563557—
반응물Diethyl(3-oxo-1,4-dioxaspiro[4.5]dec-2-yl)-phosphonateHCID 59259703—
용매TetrahydrofuranHCID 8028—
용매tert-Butyl methyl etherHCID 15413—
생성물(3E)-3-[[3,5-dimethyl-4-(phenylmethoxy)phenyl]methylene]-1,4-dioxaspiro[4.5]decan-2-oneHCID 59259697—

반응 조건

온도-20 °C

반응 단계

4.2 g lithium chloride (0.1 Mol), 20.0 g (83.2 mmol) of 4-benzyloxy-3,5-dimethylbenzaldehyde (D) and 31.62 g (108.2 mmol) of diethyl (3-oxo-1,4-dioxaspiro[4.5]dec-2-yl)-phosphonate (C) are suspended in 130 mL tetrahydrofuran and cooled to −20° C. At this temperature 12.5 mL (0.1 Mol) tetramethylguanidine are added dropwise. After the addition has ended the suspension formed is heated to ambient temperature and stirred for 1 hour. After the addition of 190 mL tert.butyl-methylether the organic phase is washed with 150 mL water and 30 mL saturated saline solution, dried and evaporated down. The resulting yellow oil is taken up in 145 mL methanol and stirred intensively for 1 hour at −10° C., during which time a white solid is formed. The solid formed is suction filtered, washed twice with 20 mL methanol/water (1:1) and dried at 45° C.

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US08119797B2
출처 데이터셋uspto-grants-2012_02
ORD IDord-9878ce2dd77a4d87abaf4743b58543bc
출처 메모uspto-grants-2012_02