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Hydrochloric Acid → 2-Methyl-L-cysteine--hydrogen chloride (1/1)

HRID 882318
ノート
印刷プレビュー

反応式

HRID 882318 の反応式
O.[ClH:2].C([S:7][CH2:8][C@@:9]([CH3:14])([C:11]([OH:13])=[O:12])[NH2:10])(C)(C)C>C(O)(C)C>[ClH:2].[CH3:14][C@@:9]([C:11]([OH:13])=[O:12])([CH2:8][SH:7])[NH2:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric Acid2 回HCID 962WaterHCID 16679762HCID 16679762、化合物

生成物 1

HCID 166797632-Methyl-L-cysteine--hydrogen chloride (1/1)収率 60%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

First, water (47.6 g) and conc. hydrochloric acid (177.4 g) were added to S-tert-butyl-α-methyl-L-cysteine (25 g, 131 mmol) produced by the method of EXAMPLE 11, and the resultant mixture was refluxed for 41 hours. Furthermore, conc. hydrochloric acid (47.6 g) was added to the mixture, followed by reflux for 3 hours. After the mixture was allowed to cool down to room temperature, isopropyl alcohol (90 mL) was added to the mixture, followed by vacuum concentration. Then, azeotropic dehydration was performed three times using the same amount of isopropyl alcohol. Finally, isopropyl alcohol was added to the residue, and the resultant mixture was concentrated to a volume of about ⅓. Then, the residue was heated to 60° C., and toluene (90 mL) was added to the residue. After the mixture was allowed to cool down to room temperature under stirring, stirring was continued about 1 hour. Then, the precipitated crystals were filtered off, washed with toluene, and dried under reduced pressure to obtain the title compound as a white solid (13.5 g, yield 60.0%).

後処理

  1. customproduced by the method of EXAMPLE 11
  2. temperatureby reflux for 3 hours
  3. concentrationfollowed by vacuum concentration
  4. additionFinally, isopropyl alcohol was added to the residue
  5. concentrationthe resultant mixture was concentrated to a volume of about ⅓
  6. temperatureThen, the residue was heated to 60° C.
  7. additiontoluene (90 mL) was added to the residue
  8. temperatureto cool down to room temperature
  9. stirringstirring
  10. filtrationThen, the precipitated crystals were filtered off
  11. washwashed with toluene
  12. customdried under reduced pressure

出典と根拠

ORDレコード
ord-acd25e42e8944ae28104e5b1ae245a22
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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