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Nitrogen → 5-(3-(6-(isopropylamino)pyrazin-2-yl)-1H-indol-5-yl)-1,2,4-oxadiazol-3-amine

HRID 634271
ノート
印刷プレビュー

反応式

HRID 634271 の反応式
I[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:11]3[O:15][N:14]=[C:13]([NH2:16])[N:12]=3)[CH:9]=2)[NH:4][CH:3]=1.[CH:17]([NH:20][C:21]1[CH:26]=[N:25][CH:24]=[C:23]([Sn](CCCC)(CCCC)CCCC)[N:22]=1)([CH3:19])[CH3:18].N#N>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH:17]([NH:20][C:21]1[N:22]=[C:23]([C:2]2[C:10]3[C:5](=[CH:6][CH:7]=[C:8]([C:11]4[O:15][N:14]=[C:13]([NH2:16])[N:12]=4)[CH:9]=3)[NH:4][CH:3]=2)[CH:24]=[N:25][CH:26]=1)([CH3:19])[CH3:18]
参加物反応条件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 947Nitrogen2 回HCID 68328197N-isopropyl-6-(tributylstannyl)pyrazin-2-amineHCID 68328272HCID 68328272、化合物

生成物 1

HCID 683289115-(3-(6-(isopropylamino)pyrazin-2-yl)-1H-indol-5-yl)-1,2,4-oxadiazol-3-amine収率 10%

試薬・触媒・溶媒 1

HCID 178418397HCID 178418397、化合物
触媒

反応条件

温度
90 °C

実験手順

To a solution of 5-(3-iodo-1H-indol-5-yl)-1,2,4-oxadiazol-3-amine (0.15 g, 0.460 mmol) and isopropyl-(6-tributylstannanyl-pyrazin-2-yl)-amine (0.235 g, 0.549 mmol) was bubbled N2 gas for 15 min. To the mixture was added Cut (0.070 g, 0.366 mmol) and Pd(PPh3)4 (0.053 g, 0.043 mmol) and N2 gas was bubbled for another 15 min. The reaction was heated at 90° C. for 1 h. The mixture was cooled to RT, quenched with H2O (100 mL) and extracted with EtOAc (2×100 mL). The organic layer was dried over anhydrous Na2SO4 and concentrated. The residue was purified with preparative HPLC (eluent: 10-60% AcCN in H2O with 0.01% TFA) to give 5-(3-(6-(isopropylamino)pyrazin-2-yl)-1H-indol-5-yl)-1,2,4-oxadiazol-3-amine (0.015 g, 10%) as a pale yellow solid. MS (ESI, pos. ion) m/z: 336.2 (M+1); 1H-NMR (400 MHz, CD3OD): δ 9.34 (s, 1H), 8.09 (s, 1H), 8.04 (d, J=0.8 Hz, 1H), 7.88 (d, J=8.4 Hz, 1H), 7.56 (d, J=8.8 Hz, 1H), 4.39 (m, 1H), 1.38 (dd, J=6.8, 1.2 Hz, 6H).

後処理

  1. customwas bubbled for another 15 min
  2. temperatureThe mixture was cooled to RT
  3. customquenched with H2O (100 mL)
  4. extractionextracted with EtOAc (2×100 mL)
  5. dry with materialThe organic layer was dried over anhydrous Na2SO4
  6. concentrationconcentrated
  7. customThe residue was purified with preparative HPLC (eluent: 10-60% AcCN in H2O with 0.01% TFA)

出典と根拠

ORDレコード
ord-80a66754b2504e1fabde8c4430001998
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09321756B2

反応ノート

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