4-Methyloxybenzyl chloride → HCID 15170715, 화합물

HRID 486880

반응식

HRID 486880 반응식
[SH:1][C:2]([CH3:13])([CH3:12])[C:3]([NH:5][C@H:6]([C:9]([OH:11])=[O:10])[CH2:7][SH:8])=[O:4].[CH3:14][O:15][C:16]1[CH:23]=[CH:22][C:19]([CH2:20]Cl)=[CH:18][CH:17]=1>C(O)C.[OH-].[Na+]>[CH3:14][O:15][C:16]1[CH:23]=[CH:22][C:19]([CH2:20][S:8][CH2:7][C@@H:6]([C:9]([OH:11])=[O:10])[NH:5][C:3](=[O:4])[C:2]([S:1][CH2:20][C:19]2[CH:22]=[CH:23][C:16]([O:15][CH3:14])=[CH:17][CH:18]=2)([CH3:13])[CH3:12])=[CH:18][CH:17]=1

참가 물질

5

반응물 2

HCID 699934-Methyloxybenzyl chlorideHCID 656604Bucillamine

생성물 1

HCID 15170715HCID 15170715, 화합물수율 67%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 14798Sodium Hydroxide용매

실험 절차

To a stirred solution of N-(2-mercapto-2-methylpropionyl)-L-cysteine (2.0 g) in ethanol(10 ml), 4N sodium hydroxide solution(7.7 ml) and paramethoxybenzyl chloride(3.0 ml) were added dropwise under ice-cooling and under nitrogen atomosphere. After the addition, the reaction mixture was stirred for 2 hours under ice-cooling and 2 hours at room temperature. The reaction mixture was concentrated in vacuo, acidified with 2N hydrochloric acid and extracted with ether. The organic layer was washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated in vacuo to give crystals. The crystals were recrystallized with ether to give 2.8 g(67%) of the titled compound.

후처리

  1. temperaturecooling and under nitrogen atomosphere
  2. additionAfter the addition
  3. concentrationThe reaction mixture was concentrated in vacuo
  4. extractionextracted with ether
  5. washThe organic layer was washed with saturated sodium chloride solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated in vacuo
  8. customto give crystals
  9. customThe crystals were recrystallized with ether

출처 및 근거

ORD 기록
ord-8fb0a75d47eb4fcebc445aca55739003
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292926

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