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Triethylamine → Tert-butyl(1-(4-(6-chloro-1,5-naphthyridin-3-yl)piperazin-1-yl)-2-methyl-1-oxopropan-2-yl)carbamate

HRID 509644
ノート
印刷プレビュー

反応式

HRID 509644 の反応式
[C:1]([O:5][C:6]([NH:8][C:9]([CH3:14])([CH3:13])[C:10]([OH:12])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.[Cl:43][C:44]1[CH:53]=[CH:52][C:51]2[C:46](=[CH:47][C:48]([N:54]3[CH2:59][CH2:58][NH:57][CH2:56][CH2:55]3)=[CH:49][N:50]=2)[N:45]=1>C(Cl)Cl>[C:1]([O:5][C:6](=[O:7])[NH:8][C:9]([CH3:14])([CH3:13])[C:10]([N:57]1[CH2:58][CH2:59][N:54]([C:48]2[CH:49]=[N:50][C:51]3[C:46]([CH:47]=2)=[N:45][C:44]([Cl:43])=[CH:53][CH:52]=3)[CH2:55][CH2:56]1)=[O:12])([CH3:2])([CH3:3])[CH3:4]
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 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 2733845N-((1,1-dimethylethoxy)carbonyl)-2-methyl-alanineHCID 866975582-Chloro-7-(piperazin-1-yl)-1,5-naphthyridine

生成物 1

HCID 88874322
Tert-butyl(1-(4-(6-chloro-1,5-naphthyridin-3-yl)piperazin-1-yl)-2-methyl-1-oxopropan-2-yl)carbamate
収率 75.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred mixture of 2-((tert-butoxycarbonyl)amino)-2-methylpropanoic acid (180 mg, 0.89 mmol, 1.5 eq), triethylamine (209 mg, 2.07 mmol, 3.5 eq) and HOBt (120 mg, 0.89 mmol, 1.5 eq) in anhydrous CH2Cl2 (10 mL), EDCI (170 mg, 0.89 mmol, 1.5 eq) was added. The resulting mixture was stirred at RT for 30 min, and then 2-chloro-7-(piperazin-1-yl)-1,5-naphthyridine (D-19) (0.59 mmol, 1.0 eq) was added. The reaction mixture was stirred at RT for 20 h, and then quenched with water (30 mL) and CH2Cl2 (15 mL), and the organic layer was separated. The organic layer was washed with brine (10 mL), dried over anhydrous Na2SO4 and filtered. The filtrate was concentrated in vacuo. The resultant residue was purified by silica gel column chromatography (2% MeOH—CH2Cl2) to afford the desired product, tert-butyl(1-(4-(6-chloro-1,5-naphthyridin-3-yl)piperazin-1-yl)-2-methyl-1-oxopropan-2-yl)carbamate (D-20) (193 mg, 75.4% yield, 2 steps). ESI-MS m/z: 434.18[M+H]+.

後処理

  1. additionwas added
  2. stirringThe reaction mixture was stirred at RT for 20 h
  3. customquenched with water (30 mL) and CH2Cl2 (15 mL)
  4. customthe organic layer was separated
  5. washThe organic layer was washed with brine (10 mL)
  6. dry with materialdried over anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated in vacuo
  9. customThe resultant residue was purified by silica gel column chromatography (2% MeOH—CH2Cl2)

出典と根拠

ORDレコード
ord-5ee72dd57c5648c4a606f1a0a272ab3a
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09096590B2

反応ノート

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