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Hydrochloric Acid → (2S,3S)-2-amino-3-methyl-valeric acid N-{2-[3-methoxy-4-(naphthalen-1-ylmethoxy)-phenyl]-ethyl}-amide

HRID 650982
ノート
印刷プレビュー

反応式

HRID 650982 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:21][CH2:22][NH:23][C:24](=[O:38])[C@@H:25]([NH:30]C(OC(C)(C)C)=O)[C@@H:26]([CH3:29])[CH2:27][CH3:28])[CH:6]=[CH:7][C:8]=1[O:9][CH2:10][C:11]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH:14]=[CH:13][CH:12]=1.Cl.O>O1CCOCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:21][CH2:22][NH:23][C:24](=[O:38])[C@@H:25]([NH2:30])[C@@H:26]([CH3:29])[CH2:27][CH3:28])[CH:6]=[CH:7][C:8]=1[O:9][CH2:10][C:11]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH:14]=[CH:13][CH:12]=1
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 AcidHCID 962WaterHCID 56999350(2S,3S)-2-(tert-butoxycarbonyl-amino)-3-methyl-valeric acid N-{2-[3-methoxy-4-(naphthalen-1-ylmethoxy)-phenyl]-ethyl}-amide

生成物 1

HCID 57011389(2S,3S)-2-amino-3-methyl-valeric acid N-{2-[3-methoxy-4-(naphthalen-1-ylmethoxy)-phenyl]-ethyl}-amide

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane
溶媒
2 回

実験手順

12.6 9 of (2S,3S)-2-(tert-butoxycarbonyl-amino)-3-methyl-valeric acid N-{2-[3-methoxy-4-(naphthalen-1-ylmethoxy)-phenyl]-ethyl}-amide are dissolved in 100 ml of dioxane. 200 ml of a 4M solution of hydrogen chloride in dioxane are added thereto. The reaction mixture is stirred at room temperature for 24 hours and then 300 ml of water are added thereto. Extraction is carried out twice using 300 ml of ethyl acetate each time. The organic phases are washed twice using 150 ml of 2N hydrochloric acid each time. The combined aqueous extracts are adjusted to a pH value of >8 by the addition of solid potassium carbonate. Extraction is carried out twice using 400 ml of tert-butyl methyl ether each time. The organic phases are combined, dried over potassium carbonate and concentrated, yielding (2S,3S)-2-amino-3-methyl-valeric acid N-{2-[3-methoxy-4-(naphthalen-1-ylmethoxy)-phenyl]-ethyl}-amide in the form of a yellow oil.

後処理

  1. extractionExtraction
  2. washThe organic phases are washed twice
  3. additionThe combined aqueous extracts are adjusted to a pH value of >8 by the addition of solid potassium carbonate
  4. extractionExtraction
  5. dry with materialdried over potassium carbonate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-c7cb782e77d34d9bbf6cfc5e29e5992c
出典データセット
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06277849B1

反応ノート

読み込み中…

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