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5-methanesulfonyl-1-methyl-1H-1,2,3,4-tetrazole → 2-(2,6-Diethylphenyl)-4-methyl-6-(1-methyl-1H-tetrazol-5-yl)-5,6,7,8-tetrahydro-1,6-naphthyridine

HRID 80828
ノート
印刷プレビュー

反応式

HRID 80828 の反応式
Cl.Cl.[CH2:3]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([CH2:11][CH3:12])[C:6]=1[C:13]1[CH:22]=[C:21]([CH3:23])[C:20]2[CH2:19][NH:18][CH2:17][CH2:16][C:15]=2[N:14]=1)[CH3:4].[CH3:24][N:25]1[C:29](S(C)(=O)=O)=[N:28][N:27]=[N:26]1>C1COCC1.[Li]CCCC.[Cl-].[Na+].O.CCOC(C)=O>[CH2:3]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([CH2:11][CH3:12])[C:6]=1[C:13]1[CH:22]=[C:21]([CH3:23])[C:20]2[CH2:19][N:18]([C:29]3[N:25]([CH3:24])[N:26]=[N:27][N:28]=3)[CH2:17][CH2:16][C:15]=2[N:14]=1)[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 2

HCID 64212595-methanesulfonyl-1-methyl-1H-1,2,3,4-tetrazoleHCID 86690277HCID 86690277、化合物

生成物 1

HCID 712404722-(2,6-Diethylphenyl)-4-methyl-6-(1-methyl-1H-tetrazol-5-yl)-5,6,7,8-tetrahydro-1,6-naphthyridine

試薬・触媒・溶媒 4

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒
HCID 57417360
Sodium chloride; water
溶媒
HCID 178418339Butyllithium溶媒

実験手順

To a solution of 2-(2,6-diethylphenyl)-4-methyl-5,6,7,8-tetrahydro-1,6-naphthyridine dihydrochloride (21.7 mg, 0.061 mmol) in THF (0.5 mL), 1.6 M n-BuLi in hexanes (0.119 mL, 0.190 mmol) was added at −78° C. under nitrogen. After stirring for 10 min. at the same temperature, 1-methyl-5-(methylsulfonyl)-1H-tetrazole (24.90 mg, 0.154 mmol) was added. The mixture was warmed up to rt and stirred for 19 h. The mixture was diluted with brine and EtOAc. The products were extracted with EtOAc, and the organic layer was concentrated. The crude was purified by RP-HPLC (X-Bridge Phenyl®, H2O (0.1% NH4OH)/CH3CN), then the fractions including the desired product were lyophilized to give the desired product. 1H NMR (400 MHz, CDCl3) δ ppm 7.26-7.30 (m, 2 H), 7.14 (d, J=7.58 Hz, 1 H), 6.98 (s, 1 H), 4.58 (s, 2 H), 4.01 (s, 3 H), 3.68 (t, J=5.94 Hz, 2 H), 3.25 (br t, J=5.94 Hz, 2 H), 2.30-2.37 (m, 7 H), 1.06 (t, J=7.58 Hz, 6 H); MS (ESI+) m/z 363.27 (M+H)+.

後処理

  1. additionwas added
  2. extractionThe products were extracted with EtOAc
  3. concentrationthe organic layer was concentrated
  4. customThe crude was purified by RP-HPLC (X-Bridge Phenyl®, H2O (0.1% NH4OH)/CH3CN)

出典と根拠

ORDレコード
ord-d8a04dedffa740b591448921b5b0c1d4
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846656B2

反応ノート

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