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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 16679760, 화합물 → HCID 16679762, 화합물

HRID 882316
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HRID 882316 반응식
C([NH:4][C@:5]([CH3:15])([C:12]([OH:14])=[O:13])[CH2:6][S:7][C:8]([CH3:11])([CH3:10])[CH3:9])(=O)N>[OH-].[Li+]>[C:8]([S:7][CH2:6][C@@:5]([CH3:15])([C:12]([OH:14])=[O:13])[NH2:4])([CH3:11])([CH3:9])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 16679760HCID 16679760, 화합물

생성물 1

HCID 16679762HCID 16679762, 화합물수율 80.2%

시약·촉매·용매 1

HCID 3939Lithium Hydroxide용매

실험 절차

N-carbamoyl-S-tert-butyl-α-methyl-L-cysteine (82.4 g, 351.4 mmol) was dissolved in a 18% aqueous lithium hydroxide solution (630 g), and the resultant solution was refluxed in nitrogen for 41 hours. After the solution was allowed to cool down to room temperature, the insoluble substance was filtered off, and the filtrate was adjusted to pH 6 by adding conc. hydrochloric acid (180.1 g). After stirring for about 1 hour, the mixture was cooled to 4° C. to 5° C., and further stirred for 1 hour. The produced crystals were filtered off, washed with water, and then dried under reduced pressure to obtain the title compound as a white solid (53.9 g). As a result of HPLC analysis (column: COSMOSIL 5C18-AR (produced by Nacalai Tesque Inc.), mobile phase: potassium dihydrogen phosphate-phosphoric acid solution (pH 2.0)/acetonitrile=90/10, flow rate: 1.0 ml/min, detection wavelength: 210 nm, column temperature: 40° C.), it was confirmed that the solid was the desired compound (yield 85.7%)

후처리

  1. filtrationthe insoluble substance was filtered off
  2. additionby adding conc. hydrochloric acid (180.1 g)
  3. temperaturethe mixture was cooled to 4° C. to 5° C.
  4. stirringfurther stirred for 1 hour
  5. filtrationThe produced crystals were filtered off
  6. washwashed with water
  7. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-3761ecc8d2a847c8be7ab8670644c8ba
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08993800B2

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