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Ammonia → N-(2-amino-2-oxo-1-phenylethyl)-3-(biphenyl-4-ylsulfonyl)-1,3-thiazolidine-2-carboxamide

HRID 1964842
ノート
印刷プレビュー

反応式

HRID 1964842 の反応式
[C:1]1([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH:6]=[CH:5][C:4]([S:7]([N:10]2[CH2:14][CH2:13][S:12][CH:11]2[C:15]([NH:17][CH:18]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:19](O)=[O:20])=[O:16])(=[O:9])=[O:8])=[CH:3][CH:2]=1.[NH3:34].O1CCOCC1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl>C1COCC1.CN(C1C=CN=CC=1)C.CCOC(C)=O>[NH2:34][C:19](=[O:20])[CH:18]([NH:17][C:15]([CH:11]1[N:10]([S:7]([C:4]2[CH:3]=[CH:2][C:1]([C:28]3[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=3)=[CH:6][CH:5]=2)(=[O:9])=[O:8])[CH2:14][CH2:13][S:12]1)=[O:16])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 222AmmoniaHCID 312751,4-DioxaneHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 10128046({[3-(Biphenyl-4-ylsulfonyl)-1,3-thiazolidin-2-yl]carbonyl}amino)(phenyl)acetic acid

生成物 1

HCID 10288863
N-(2-amino-2-oxo-1-phenylethyl)-3-(biphenyl-4-ylsulfonyl)-1,3-thiazolidine-2-carboxamide
収率 80%

試薬・触媒・溶媒 3

HCID 142844-(Dimethylamino)pyridine触媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Compound Ia, e.g., ({[3-(biphenyl-4-ylsulfonyl)-1,3-thiazolidin-2-yl]carbonyl}amino)-(phenyl)acetic acid (500 mg, 1.04 mmol) was dissolved in THF (10 mL). Ammonia in dioxane (0.5N, 3.11 mL, 1.55 mmol) was added followed by HOBt (210 mg, 1.55 mmol) and DMAP (6 mg, 0.05 mmol). EDC.HCl (298 mg, 1.55 mmol) was finally added. The mixture was stirred for 5 hours at RT. As the reaction was complete, it was diluted with EtOAc, washed with 5% citric acid, NH4Cl sat, NaHCO3 sat, brine and dried over MgSO4. After filtration and evaporation of the solvents, the resulting crude product was purified by flash chromatography (Cyclohexane/EtOAc, gradient from 1:1 to 0:1). Compound Ib, e.g. N-(2-amino-2-oxo-1-phenylethyl)-3-(biphenyl-4-ylsulfonyl)-1,3-thiazolidine-2-carboxamide, was isolated in 90% purity by HPLC (349 mg, 80% yield).

後処理

  1. washwashed with 5% citric acid, NH4Cl
  2. dry with materialbrine and dried over MgSO4
  3. filtrationAfter filtration and evaporation of the solvents
  4. customthe resulting crude product was purified by flash chromatography (Cyclohexane/EtOAc, gradient from 1:1 to 0:1)

出典と根拠

ORDレコード
ord-d2948a529924486ca6d60a648d3e4907
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08415480B2

反応ノート

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