Diisopropylethylamine → HCID 135800728, 화합물

HRID 1247778노트

반응식

HRID 1247778 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 135800728HCID 135800728, 화합물수율 74.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e112db3312f442418e87c290c9d8517b
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07129232B2

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