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HCID 16679760、化合物 → HCID 16679762、化合物

HRID 882316
ノート
印刷プレビュー

反応式

HRID 882316 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 16679760HCID 16679760、化合物

生成物 1

HCID 16679762HCID 16679762、化合物収率 80.2%

試薬・触媒・溶媒 1

HCID 3939Lithium Hydroxide溶媒

実験手順

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%)

後処理

  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

出典と根拠

ORDレコード
ord-3761ecc8d2a847c8be7ab8670644c8ba
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08993800B2

反応ノート

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