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Hydrochloric Acid → (S)-3-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-yl]-2-[2-ethyl-3-(3-oxo-morpholin-4-yl)-benzenesulfonylamino]-propionic acid

HRID 76802
ノート
印刷プレビュー

反応式

HRID 76802 の反応式
C[O:2][C:3](=[O:36])[C@@H:4]([NH:17][S:18]([C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([N:27]2[CH2:32][CH2:31][O:30][CH2:29][C:28]2=[O:33])[C:22]=1[CH2:34][CH3:35])(=[O:20])=[O:19])[CH2:5][C:6]1[CH:10]=[C:9]([C:11]2[S:12][C:13]([Cl:16])=[CH:14][CH:15]=2)[O:8][N:7]=1.[Li+].[OH-].Cl>C1COCC1.CO.O>[Cl:16][C:13]1[S:12][C:11]([C:9]2[O:8][N:7]=[C:6]([CH2:5][C@H:4]([NH:17][S:18]([C:21]3[CH:26]=[CH:25][CH:24]=[C:23]([N:27]4[CH2:32][CH2:31][O:30][CH2:29][C:28]4=[O:33])[C:22]=3[CH2:34][CH3:35])(=[O:20])=[O:19])[C:3]([OH:36])=[O:2])[CH:10]=2)=[CH:15][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 66911103(S)-3-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-yl]-2-[2-ethyl-3-(3-oxo-morpholin-4-yl)-benzenesulfonylamino]-propionic acid methyl ester

生成物 1

HCID 66911167(S)-3-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-yl]-2-[2-ethyl-3-(3-oxo-morpholin-4-yl)-benzenesulfonylamino]-propionic acid

試薬・触媒・溶媒 3

HCID 887
Methanol
溶媒
HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

Intermediate 7 (1.5 g, 2.71 mmol) in THF (15 ml), MeOH (5 ml) and water (5 ml) was treated with LiOH (194 mg, 8.12 mmol) and stirred at RT overnight. The mixture was acidified with HCl and extracted with ethyl acetate. The combined organic layers were washed with water and brine, dried with MgSO4, filtered and evaporated to dryness. The crude product (1.3 g) was used without further purification in the next step.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe combined organic layers were washed with water and brine
  3. dry with materialdried with MgSO4
  4. filtrationfiltered
  5. customevaporated to dryness
  6. customThe crude product (1.3 g) was used without further purification in the next step

出典と根拠

ORDレコード
ord-bbeba29e22a04a3a98f40a2768309dc9
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08835653B2

反応ノート

読み込み中…

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