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4-Methylmorpholine → Ethyl 2-[3-(5,6,7,8-tetrahydro-[1,8]naphthyridin-2-yl)-propylcarbamoyl]-acetate

HRID 617903
ノート
印刷プレビュー

反応式

HRID 617903 の反応式
[N:1]1[C:10]2[NH:9][CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][C:2]=1[CH2:11][CH2:12][CH2:13][NH2:14].C([CH:17]([C:21]([OH:23])=O)[C:18]([OH:20])=[O:19])C.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)[C:35]2C=CC=C[C:34]=2N=N1.CN1CCOCC1>CN(C=O)C.C(OCC)(=O)C>[N:1]1[C:10]2[NH:9][CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][C:2]=1[CH2:11][CH2:12][CH2:13][NH:14][C:21]([CH2:17][C:18]([O:20][CH2:34][CH3:35])=[O:19])=[O:23]
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 4

HCID 79724-MethylmorpholineHCID 11756Ethylmalonic acidHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 98775993-(5,6,7,8-Tetrahydro-1,8-naphthyridin-2-yl)propan-1-amine

生成物 1

HCID 21850003Ethyl 2-[3-(5,6,7,8-tetrahydro-[1,8]naphthyridin-2-yl)-propylcarbamoyl]-acetate

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 1-8 (0.068 g, 0.36 mmol), ethylmalonic acid (0.052 g, 0.40 mmol), BOP (0.24 g, 0.54 mmol), and NMM (0.16 mL, 1.4 mmol) in DMF (1.8 mL) was stirred at ambient temperature for 20 h. The mixture was diluted with ethyl acetate, washed with water, brine, and dried over MgSO4. Following evaporative removal of the solvent, the residue was chromatographed on silica gel, eluting with 15% ethanol/EtOAc to give 1-9 as a colorless glass.

後処理

  1. washwashed with water, brine
  2. dry with materialdried over MgSO4
  3. customremoval of the solvent
  4. customthe residue was chromatographed on silica gel
  5. washeluting with 15% ethanol/EtOAc

出典と根拠

ORDレコード
ord-532b10e154474506ac8549ea4b856d4a
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05952341

反応ノート

読み込み中…

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