Water → Methyl 2-trimethylsilylacetylene 2-carbethoxyaminoacetate

HRID 371956

반응식

HRID 371956 반응식
[C:1]([NH:6][CH:7](Cl)[C:8]([O:10]C)=[O:9])([O:3][CH2:4][CH3:5])=[O:2].[CH3:13][Si:14]([C:17]#[C:18][Si](C)(C)C)([CH3:16])[CH3:15].[Cl-].[Al+3].[Cl-].[Cl-].O>C(Cl)Cl>[CH3:1][C:18]#[C:17][Si:14]([CH3:16])([CH3:15])[CH3:13].[C:1]([NH:6][CH2:7][C:8]([O-:10])=[O:9])([O:3][CH2:4][CH3:5])=[O:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 84564Bis(trimethylsilyl)acetyleneHCID 6451240Aluminum(III) ChlorideHCID 15571344methyl N-carbethoxy-2-chloroglycinate

생성물 1

HCID 86735698Methyl 2-trimethylsilylacetylene 2-carbethoxyaminoacetate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
25 °C

실험 절차

To 19.5 g (0.1 M) of methyl N-carbethoxy-2-chloroglycinate and 17.0 g (0.1 M) of bis-trimethylsilyl acetylene in 200 ml of methylene chloride at 0° C is added 13.5 g (0.1 M) of aluminum chloride and the reaction mixture is allowed to warm to 25° C. After 24 hours at 25° C water is carefully added to the mixture which is then extracted with methylene chloride. The combined organic solutions are dried over magnesium sulfate, concentrated and distilled with the b.p. 100°/0.15 mm fraction collected to give methyl 2-trimethylsilylacetylene-2-carbethoxyaminoacetate.

후처리

  1. extractionis then extracted with methylene chloride
  2. dry with materialThe combined organic solutions are dried over magnesium sulfate
  3. concentrationconcentrated
  4. distillationdistilled with the b.p. 100°/0.15 mm fraction
  5. customcollected

출처 및 근거

ORD 기록
ord-5a21285654ca41feb8eb945e6b016e70
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04088667

연결된 노트

불러오는 중…