Isobutyraldehyde → Methyl 2,2,4-trimethyl-3-trimethylsiloxyvalerate

HRID 544260

반응식

HRID 544260 반응식
[C:1]([O-])(=[O:6])CCCC.[CH:8](=[O:12])[CH:9]([CH3:11])[CH3:10].CO[C:15]([O:19][Si:20]([CH3:23])([CH3:22])[CH3:21])=[C:16]([CH3:18])[CH3:17].C(OCC)(=O)C>O1CCCC1>[CH3:10][C:9]([CH3:11])([CH:15]([O:19][Si:20]([CH3:21])([CH3:22])[CH3:23])[CH:16]([CH3:17])[CH3:18])[C:8]([O:6][CH3:1])=[O:12]

참가 물질

6

반응물 4

HCID 6561IsobutyraldehydeHCID 8857Ethyl AcetateHCID 114781ValerateHCID 552336Silane, ((1-methoxy-2-methyl-1-propenyl)oxy)trimethyl-

생성물 1

HCID 14763594Methyl 2,2,4-trimethyl-3-trimethylsiloxyvalerate수율 97%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In another preparation of the aforesaid valerate, isobutyraldehyde (0.72 g) was added to a mixture of [(1-methoxy-2-methyl-1-propenyl)oxy]trimethylsilane (1.74 g, 10 mmol) and (TAS)HF2 (100 mg, 0.1 mmol) in 20 mL of tetrahydrofuran under argon at -11°. The reaction mixture was stirred and the temperature was allowed to rise to 23°. Stirring was continued for 18 h and the mixture was then poured into 200 mL of ethyl acetate and extracted with water (200 mL), followed by washing with aqueous brine (200 mL). The organic layer was dried (MgSO4), filtered and evaporated in vacuo to give 2.39 g (97% yield) of methyl 2,2,4-trimethyl-3-trimethylsiloxyvalerate.

후처리

  1. customto rise to 23°
  2. stirringStirring
  3. extractionextracted with water (200 mL)
  4. washby washing with aqueous brine (200 mL)
  5. dry with materialThe organic layer was dried (MgSO4)
  6. filtrationfiltered
  7. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-bac238b4f8af48f1ab9eab24db71a069
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04448980

연결된 노트

불러오는 중…