Diisopropylethylamine → HCID 135800728、化合物

HRID 1247778ノート

反応式

HRID 1247778 の反応式
S(=O)(=O)(O)O.[NH2:6][C:7]1[CH:11]=[N:10][N:9]2[CH2:12][CH2:13][NH:14][C:8]=12.C(N(C(C)C)C(C)C)C.[C:24]([O:28][C:29]([NH:31][CH2:32][CH2:33][C:34](ON1C(=O)CCC1=O)=[O:35])=[O:30])([CH3:27])([CH3:26])[CH3:25]>C(Cl)Cl>[C:24]([O:28][C:29]([NH:31][CH2:32][CH2:33][C:34]([NH:6][C:7]1[CH:11]=[N:10][N:9]2[CH2:12][CH2:13][NH:14][C:8]=12)=[O:35])=[O:30])([CH3:27])([CH3:26])[CH3:25]

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 10684599Boc-Beta-Ala-OSuHCID 1358007252,3-dihydro-1H-imidazo[1,2-b]pyrazol-7-amine sulfate

生成物 1

HCID 135800728HCID 135800728、化合物収率 74.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 7-amino-2,3-dihydro-1H-imidazo[1,2-b]pyrazole sulfuric acid salt (2.22 g) and N-ethyldiisopropylamine (2.84 g) in methylene chloride (70 ml) was added N-[3-(tert-butoxycarbonylamino)propionyloxy]succinimide (3.15 g). The mixture was stirred at room temperature for 4 hours. The reaction mixture was washed with saturated aqueous sodium hydrogen carbonate solution, and the organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The oily residue was purified by column chromatography on silica gel eluting with 5% methanol/chloroform to give 7-[3-(tert-butoxycarbonylamino)propionyl]amino-2,3-dihydro-1H-imidazo[1,2-b]pyrazole (2.2 g) as a solid.

後処理

  1. washThe reaction mixture was washed with saturated aqueous sodium hydrogen carbonate solution
  2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe oily residue was purified by column chromatography on silica gel eluting with 5% methanol/chloroform

出典と根拠

ORDレコード
ord-e112db3312f442418e87c290c9d8517b
出典データセット
uspto-grants-2006_10
特許番号
US07129232B2

反応ノート

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