Sulfuric Acid → methyl (S)-3-t-butoxy-2-methylpropionate

HRID 654988노트

반응식

HRID 654988 반응식
[CH3:1][C@@H:2]([CH2:7][OH:8])[C:3]([O:5][CH3:6])=[O:4].S(=O)(=O)(O)O.[CH2:14]=[C:15]([CH3:17])[CH3:16]>ClCCl>[C:15]([O:8][CH2:7][C@H:2]([CH3:1])[C:3]([O:5][CH3:6])=[O:4])([CH3:17])([CH3:16])[CH3:14]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 8255IsobutyleneHCID 10192563methyl (2S)-3-hydroxy-2-methylpropanoate

생성물 1

HCID 12923319methyl (S)-3-t-butoxy-2-methylpropionate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Methyl (S)-(+)-2-methyl-3-hydroxypropionate (2.36 g; 20 mmole) was dissolved in dry dichloromethane (30 ml), conc. sulfuric acid (0.2 ml) was added thereto, and isobutene (23.5 g) was introduced into the resultant mixture kept at -60° to -70° C., followed by stirring at room temperature for 3 hours. The reaction mixture was sealed and stirred overnight, and unreacted isobutene was removed therefrom by distillation. The mixture was washed successively with water and a saturated sodium bicarbonate solution, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give methyl (S)-3-t-butoxy-2-methylpropionate.

후처리

  1. customkept at -60° to -70° C.
  2. customThe reaction mixture was sealed
  3. stirringstirred overnight
  4. customunreacted isobutene was removed
  5. distillationby distillation
  6. washThe mixture was washed successively with water
  7. dry with materiala saturated sodium bicarbonate solution, dried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-528ad113cd784dd0a1c7ffb59f6cf9e4
출처 데이터셋
uspto-grants-1992_07
특허 번호
US05134231

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