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1,2-Dichloroethane → 3-(5-5,6,7,8-Tetrahydro-[1,8]naphthyridin-2-yl-pentanoylamino)-propionic acid

HRID 1837899
ノート
印刷プレビュー

反応式

HRID 1837899 の反応式
Cl.[N:2]1[C:11]2[NH:10][CH2:9][CH2:8][CH2:7][C:6]=2[CH:5]=[CH:4][C:3]=1[CH2:12][CH2:13][CH2:14][CH2:15][C:16]([OH:18])=O.C(Cl)CCl.C1C=CC2N([OH:32])N=NC=2C=1.C[N:34]1[CH2:39][CH2:38]OCC1.CN([CH:43]=[O:44])C>C(OCC)(=O)C>[N:2]1[C:11]2[NH:10][CH2:9][CH2:8][CH2:7][C:6]=2[CH:5]=[CH:4][C:3]=1[CH2:12][CH2:13][CH2:14][CH2:15][C:16]([NH:34][CH2:39][CH2:38][C:43]([OH:44])=[O:32])=[O:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 111,2-DichloroethaneHCID 6228DimethylformamideHCID 79724-MethylmorpholineHCID 757711-HydroxybenzotriazoleHCID 697750595-(5,6,7,8-Tetrahydro-1,8-naphthyridin-2-yl)pentanoic acid hydrochloride

生成物 1

HCID 99011043-(5-5,6,7,8-Tetrahydro-[1,8]naphthyridin-2-yl-pentanoylamino)-propionic acid

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of acid 1-6 (10.8 mg, 0.04 mmol), EDC (7.7 mg, 0.04 mmol), HOBT (5.4 mg, 0.04 mmol) and NMM (0.026 mL, 0.24 mmol) in DMF (1 mL) was agitated until clear solution. After 30 minutes, amine 12-1 was added. The solution was agitated for one minute and then let stand for 18 h. The solution was diluted with ethyl acetate, washed with sat. NaHCO3 and H2O. Following evaporative removal of the solvent, the residue was dissolved in 90:10 TFA/H2O (1 ml). After 2 h, the solvents were evaporated to give acid 12-2.

後処理

  1. stirringThe solution was agitated for one minute
  2. waitlet stand for 18 h
  3. washwashed with sat. NaHCO3 and H2O
  4. customremoval of the solvent
  5. dissolutionthe residue was dissolved in 90:10 TFA/H2O (1 ml)
  6. waitAfter 2 h
  7. customthe solvents were evaporated

出典と根拠

ORDレコード
ord-4abd890d8ead460dae98a8df4c6230a2
出典データセット
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06784190B2

反応ノート

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