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Potassium Carbonate → 6-[2-(4-cyclobutylpiperazin-1-yl)-2-oxoethyl]-5,6,7,8-tetrahydro-1,6-naphthyridin-2(1H)-one

HRID 1713120
ノート
印刷プレビュー

反応式

HRID 1713120 の反応式
[NH:1]1[C:10]2[CH2:9][CH2:8][NH:7][CH2:6][C:5]=2[CH:4]=[CH:3][C:2]1=[O:11].Cl[CH2:13][C:14]([N:16]1[CH2:21][CH2:20][N:19]([CH:22]2[CH2:25][CH2:24][CH2:23]2)[CH2:18][CH2:17]1)=[O:15].C([O-])([O-])=O.[K+].[K+]>CC#N>[CH:22]1([N:19]2[CH2:20][CH2:21][N:16]([C:14](=[O:15])[CH2:13][N:7]3[CH2:8][CH2:9][C:10]4[NH:1][C:2](=[O:11])[CH:3]=[CH:4][C:5]=4[CH2:6]3)[CH2:17][CH2:18]2)[CH2:25][CH2:24][CH2:23]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 210711895,6,7,8-Tetrahydro-1,6-naphthyridin-2(1H)-oneHCID 574205621-(Chloroacetyl)-4-cyclobutylpiperazine

生成物 1

HCID 574206516-[2-(4-cyclobutylpiperazin-1-yl)-2-oxoethyl]-5,6,7,8-tetrahydro-1,6-naphthyridin-2(1H)-one

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 5,6,7,8-tetrahydro-1,6-naphthyridin-2(1H)-one (98 mg, 0.653 mmol), 1-(chloroacetyl)-4-cyclobutylpiperazine (142 mg, 0.653 mmol), K2CO3 (360 mg, 2.61 mmol) and KI (12 mg, 0.07 mmol) in CH3CN (15 mL) is stirred at rt overnight. The solvent is removed in vacuo and the residue is partitioned between water (10 mL) and EtOAc (20 mL). The layers are separated and the aqueous layer is extracted with EtOAc (2×10 mL) and the combined extracts are dried and evaporated. The resulting oil is purified by PTLC with DCM/MeOH/NH4OH (100:5:0.5) to give the title compound as a light yellow solid. MS (M+1): 331.2; 1H NMR (δ, CDCl3): 7.13 (d, 1H0, 6.38 (d, 1H), 3.60 (q, 4H), 3.44 (s, 2H), 3.35 (s, 2H), 2.79 (s, 2H), 2.63-2.75 (m, 1H), 2.26 (q, 4H), 1.63-2.06 (m, 6H).

後処理

  1. customThe solvent is removed in vacuo
  2. customthe residue is partitioned between water (10 mL) and EtOAc (20 mL)
  3. customThe layers are separated
  4. extractionthe aqueous layer is extracted with EtOAc (2×10 mL)
  5. customthe combined extracts are dried
  6. customevaporated
  7. customThe resulting oil is purified by PTLC with DCM/MeOH/NH4OH (100:5:0.5)

出典と根拠

ORDレコード
ord-3c050de42b0a473cb88e65134c508eca
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07795262B2

反応ノート

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