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Diisopropylethylamine → (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

HRID 76801
ノート
印刷プレビュー

反応式

HRID 76801 の反応式
[CH3:1][O:2][C:3](=[O:18])[C@@H:4]([NH2:17])[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.CCN(C(C)C)C(C)C.[CH2:28]([C:30]1[C:35]([N:36]2[CH2:41][CH2:40][O:39][CH2:38][C:37]2=[O:42])=[CH:34][CH:33]=[CH:32][C:31]=1[S:43](Cl)(=[O:45])=[O:44])[CH3:29]>C(Cl)Cl>[CH3:1][O:2][C:3](=[O:18])[C@@H:4]([NH:17][S:43]([C:31]1[CH:32]=[CH:33][CH:34]=[C:35]([N:36]2[CH2:41][CH2:40][O:39][CH2:38][C:37]2=[O:42])[C:30]=1[CH2:28][CH3:29])(=[O:45])=[O:44])[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
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 81531Diisopropylethylamine2 回HCID 66911101(S)-2-Amino-3-[5-(5-chloro-thiophen-2-yl)-isoxazol-3-yl]-propionic acid methyl esterHCID 727928892-Ethyl-3-(3-oxomorpholino)benzene-1-sulfonyl chloride2 回

生成物 1

HCID 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

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

実験手順

Intermediate 2 (860 mg, 3 mmol) was dissolved in 15 ml DCM and DIPEA (2.041 ml, 12 mmol). 2-ethyl-3-(3-oxo-morpholin-4-yl)-benzenesulfonyl chloride, Intermediate 6 (911 mg, 3 mmol) in 10 ml DCM was slowly added and the reaction was stirred at RT overnight. After that 300 μl DIPEA were added and the reaction mixture was heated to 40° C. for 30 min. Then the solution was evaporated to dryness, dissolved in ethyl acetate, washed with 1 N HCl, sat. aq. NaHCO3 and brine. The combined organic layers were dried with MgSO4, filtered and evaporated to dryness. The crude product (1.5 g) was used without further purification in the next step.

後処理

  1. temperaturethe reaction mixture was heated to 40° C. for 30 min
  2. customThen the solution was evaporated to dryness
  3. dissolutiondissolved in ethyl acetate
  4. washwashed with 1 N HCl, sat. aq. NaHCO3 and brine
  5. dry with materialThe combined organic layers were dried with MgSO4
  6. filtrationfiltered
  7. customevaporated to dryness
  8. customThe crude product (1.5 g) was used without further purification in the next step

出典と根拠

ORDレコード
ord-b2961fd5834e4dc08ce0b2adb3a03e54
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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