Benzyl Alcohol → HCID 86735353, 화합물

HRID 838963노트

반응식

HRID 838963 반응식
[C:1]([O:5][C:6](=[O:13])[CH2:7][NH:8][CH2:9][CH2:10][O:11][CH3:12])([CH3:4])(C)C.C(O)[C:15]1[CH:20]=[CH:19]C=[CH:17][CH:16]=1.O.[C:23]1([CH3:33])[CH:28]=[CH:27][C:26]([S:29]([OH:32])(=[O:31])=[O:30])=[CH:25][CH:24]=1.O>C1C=CC=CC=1>[C:23]1([CH3:33])[CH:24]=[CH:25][C:26]([S:29]([OH:32])(=[O:30])=[O:31])=[CH:27][CH:28]=1.[CH2:1]([O:5][C:6](=[O:13])[CH2:7][NH:8][CH2:9][CH2:10][O:11][CH3:12])[C:4]1[CH:19]=[CH:20][CH:15]=[CH:16][CH:17]=1

참가 물질

6

반응물 4

HCID 244Benzyl AlcoholHCID 962Water2회HCID 521998p-Toluenesulfonic acid monohydrateHCID 18925475Tert-butyl 2-((2-methoxyethyl)amino)acetate

생성물 1

HCID 86735353HCID 86735353, 화합물수율 85.1%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a solution of 55.8 g of N-(2-methoxyethyl)glycine tert-butyl ester in 200 ml of benzene was added 63.8 g of benzyl alcohol and 72.9 g of p-toluenesulfonic acid monohydrate. The mixture was heated at reflux for 10 hours with the continuous removal of water through a Dean-Stark water trap. At the end of this period, the solution was concentrated in vacuo, and to the residue was added 300 ml of dry ethyl ether. After 2 hours at room temperature, the formed precipitate was filtered, washed with dry ethyl ether and then recrystallized from ethyl acetate to yield 99.2 g (85 percent) of N-(2-methoxyethyl)glycine benzyl ester p-toluenesulfonate, M.P. 95°-96° C.

후처리

  1. temperatureThe mixture was heated
  2. concentrationAt the end of this period, the solution was concentrated in vacuo
  3. additionto the residue was added 300 ml of dry ethyl ether
  4. filtrationthe formed precipitate was filtered
  5. washwashed with dry ethyl ether
  6. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-c7f4ca08a6b345bab5e4f4aad208d408
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04093712

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