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Hydrochloric Acid → HCID 12096027、化合物

HRID 1793954
ノート
印刷プレビュー

反応式

HRID 1793954 の反応式
Cl.[NH2:2][CH2:3][CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[C:10]([C:12]1[CH:13]=[CH:14][C:15]([OH:38])=[C:16]([S:18]([NH:21][CH2:22][CH2:23][C:24]2[CH:29]=[CH:28][C:27]([CH:30]([CH3:32])[CH3:31])=[CH:26][C:25]=2[NH:33][CH2:34][C:35](O)=[O:36])(=[O:20])=[O:19])[CH:17]=1)#[N:11].O.ON1C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC.Cl>CN(C)C=O.C(N(CC)CC)C>[C:10]([C:12]1[CH:13]=[CH:14][C:15]([OH:38])=[C:16]([S:18]([NH:21][CH2:22][CH2:23][C:24]2[CH:29]=[CH:28][C:27]([CH:30]([CH3:32])[CH3:31])=[CH:26][C:25]=2[NH:33][CH2:34][C:35]([NH:2][CH2:3][CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])=[O:36])(=[O:19])=[O:20])[CH:17]=1)#[N:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 458475beta-Alanine, ethyl ester, hydrochlorideHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 12096026[[2-[2-(5-Cyano-2-hydroxybenzenesulfonylamino)ethyl]-5-isopropylphenyl]amino]acetic acid

生成物 1

HCID 12096027
HCID 12096027、化合物
収率 75.1%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8471Triethylamine溶媒

実験手順

To a stirred solution of 0.11 g of ethyl 3-aminopropionate hydrochloride in 10 mL of N,N-dimethylformamide were added 0.072 ml of triethylamine, 0.30 g of [[2-[2-(5-cyano-2-hydroxybenzenesulfonylamino)ethyl]-5-isopropylphenyl]amino]acetic acid, and 0.121 g of 1-hydroxybenzotriazole monohydrate under ice-cooling, and the mixture was stirred at 5minutes. To the mixture was added 0.140 g of 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride under the same condition, and the mixture was stirred at room temperature for 7 hours. To the reaction mixture was added 1 mol/L hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: ethyl acetate-hexane) to give 0.278 g of ethyl 3-[2-[[2-[2-(5-cyano-2-hydroxybenzenesulfonylamino)ethyl]-5-isopropylphenyl]amino]acetylamino]propionate.

後処理

  1. temperaturecooling
  2. stirringthe mixture was stirred at room temperature for 7 hours
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was removed under reduced pressure
  7. customthe residue was purified by column chromatography on silica gel (eluent: ethyl acetate-hexane)

出典と根拠

ORDレコード
ord-4b6ee67f1b294085a2108de2229a148d
出典データセット
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07022689B2

反応ノート

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