Isovaleryl chloride → HCID 57675214、化合物

HRID 490919ノート

反応式

HRID 490919 の反応式
[C:1](Cl)(=[O:6])[CH2:2][CH:3]([CH3:5])[CH3:4].Cl.[CH2:9]([N:11]1[C:15]2[N:16]=[CH:17][C:18]([C:27]3[O:31][N:30]=[C:29]([CH2:32][CH:33]4[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]4)[N:28]=3)=[C:19]([NH:20][CH:21]3[CH2:26][CH2:25][O:24][CH2:23][CH2:22]3)[C:14]=2[CH:13]=[N:12]1)[CH3:10].C(N(C(C)C)CC)(C)C>C(Cl)(Cl)Cl>[CH2:9]([N:11]1[C:15]2[N:16]=[CH:17][C:18]([C:27]3[O:31][N:30]=[C:29]([CH2:32][CH:33]4[CH2:38][CH2:37][N:36]([C:1](=[O:6])[CH2:2][CH:3]([CH3:5])[CH3:4])[CH2:35][CH2:34]4)[N:28]=3)=[C:19]([NH:20][CH:21]3[CH2:22][CH2:23][O:24][CH2:25][CH2:26]3)[C:14]=2[CH:13]=[N:12]1)[CH3:10]

参加物

5

反応物 3

HCID 66054Isovaleryl chlorideHCID 81531DiisopropylethylamineHCID 67529443HCID 67529443、化合物

生成物 1

HCID 57675214HCID 57675214、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Isovaleryl chloride (0.04 mmol) was added to a stirred solution of Intermediate 125 (0.033 mmol) and diisopropylethylamine (0.1 mmol) in chloroform (1 ml) at room temperature. After stirring at room temperature for 1.5 h, the reaction mixture was applied to a SPE cartridge (aminopropyl, 1 g) and the cartridge was eluted sequentially with chloroform, ethyl acetate and methanol. Fractions containing the desired product were combined and blown down under nitrogen. The resulting residue was further purified on a SPE cartridge (silica, 1 g) eluting with a gradient of 30-100% ethyl acetate in petroleum ether to afford Example 176. LCMS showed MH+=496, TRET=3.17 min.

後処理

  1. washthe cartridge was eluted sequentially with chloroform, ethyl acetate and methanol
  2. additionFractions containing the desired product
  3. customThe resulting residue was further purified on a SPE cartridge (silica, 1 g)
  4. washeluting with a gradient of 30-100% ethyl acetate in petroleum ether
  5. customto afford Example 176
  6. customMH+=496, TRET=3.17 min.

出典と根拠

ORDレコード
ord-f03eda8da05b43dd84fd8d0945ad6999
出典データセット
uspto-grants-2009_05
特許番号
US07528148B2

反応ノート

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