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Hydrochloric Acid → HCID 54768029、化合物

HRID 1914863
ノート
印刷プレビュー

反応式

HRID 1914863 の反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]2[O:11][C:12]3[CH:18]=[CH:17][C:16]([NH2:19])=[CH:15][C:13]=3[N:14]=2)=[CH:5][CH:4]=1)[CH3:2].[C:20]1([CH2:26][C:27](Cl)=[O:28])[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C(N(CC)C(C)C)(C)C.Cl>CN(C=O)C>[CH2:1]([C:3]1[CH:4]=[CH:5][C:6]([NH:9][C:10]2[O:11][C:12]3[CH:18]=[CH:17][C:16]([NH:19][C:27](=[O:28])[CH2:26][C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=4)=[CH:15][C:13]=3[N:14]=2)=[CH:7][CH:8]=1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7679Phenylacetyl chlorideHCID 81531DiisopropylethylamineHCID 54768028HCID 54768028、化合物

生成物 1

HCID 54768029HCID 54768029、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The compound 1 prepared in Example 1 (1 mmol, 1 eq) was dissolved with DMF (dimethylformamide, 3 mL), and 2-phenylacetyl chloride (1 mmol, 1 eq) and N,N-diisopropylethylamine (1 mmol, 1 eq) were added together thereto. The mixture was then stirred at room temperature for 16 hours. To the reaction solution was added 10% aqueous HCl solution, and the mixture was extracted with 30 mL of EtOAc. The organic layer was washed with 10% aqueous HCl solution, and then two times with saturated NaHCO3 solution and two times with saturated aqueous NaCl solution. After drying with anhydrous MgSO4 and filtering under reduced pressure, the organic solvent was removed under reduced pressure to prepare the title compound.

後処理

  1. additionwere added together
  2. extractionthe mixture was extracted with 30 mL of EtOAc
  3. washThe organic layer was washed with 10% aqueous HCl solution
  4. dry with materialAfter drying with anhydrous MgSO4
  5. filtrationfiltering under reduced pressure
  6. customthe organic solvent was removed under reduced pressure
  7. customto prepare the title compound

出典と根拠

ORDレコード
ord-7b780679f3ab4ca2b0413b41336ee981
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08614240B2

反応ノート

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