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Hydrochloric Acid → HCID 178499132、化合物

HRID 869728
ノート
印刷プレビュー

反応式

HRID 869728 の反応式
C(OC([NH:8][C@H:9]([C:11]([NH:13][C@@H:14]([C:19](=O)[CH3:20])[C:15]([O:17][CH3:18])=[O:16])=[O:12])[CH3:10])=O)(C)(C)C.Cl>O1CCOCC1>[OH:12][C:11]1[N:13]=[C:14]([C:15]([O:17][CH3:18])=[O:16])[C:19]([CH3:20])=[N:8][C:9]=1[CH3:10]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 86674523methyl (2S)-2-{[N-(tert-butoxycarbonyl)-L-alanyl]amino}-3-oxobutanoate

生成物 1

HCID 178499132HCID 178499132、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

A solution of methyl (2S)-2-{[N-(tert-butoxycarbonyl)-L-alanyl]amino}-3-oxobutanoate (3.05 g, 10.1 mmol) and 4N hydrochloric acid in 1,4-dioxane (10 mL) was stirred at room temperature. After being stirred for 1 h at same temperature, the reaction mixture was concentrated in vacuo. A solution of the residue in pyridine (50 mL) was heated at 60° C. for 4 h. After being cooled to ambient temperature, the mixture was concentrated in vacuo. The residue was poured into water, and the mixture was extracted with dichloromethane. The organic layer was washed with saturated brine, dried over magnesium sulfate, filtrated and concentrated in vacuo. The residue was triturated with hexane-ethyl acetate (1:1) to give methyl 6-hydroxy-3,5-dimethylpyrazine-2-carboxylate. MS (APCI): m/z 183 (M+H).

後処理

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. temperatureAfter being cooled to ambient temperature
  3. concentrationthe mixture was concentrated in vacuo
  4. additionThe residue was poured into water
  5. extractionthe mixture was extracted with dichloromethane
  6. washThe organic layer was washed with saturated brine
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltrated
  9. concentrationconcentrated in vacuo
  10. customThe residue was triturated with hexane-ethyl acetate (1:1)

出典と根拠

ORDレコード
ord-08c8b399f72e42feab2cd18ef302586f
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08969376B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート