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Sodium Bisulfite → HCID 178429876、化合物

HRID 1047571
ノート
印刷プレビュー

反応式

HRID 1047571 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[N:9]([CH:13]1[CH2:18][CH2:17][CH2:16][CH2:15][O:14]1)[N:8]=[C:7]2[CH:19]=O)([O-:3])=[O:2].[CH3:21][CH:22]1[CH2:27][N:26]([C:28]2[CH:29]=[C:30]([NH2:35])[C:31]([NH2:34])=[CH:32][CH:33]=2)[CH2:25][CH2:24][O:23]1.S(=O)(O)[O-].[Na+]>C1COCC1.Cl.C(OCC)(=O)C>[CH3:21][CH:22]1[O:23][CH2:24][CH2:25][N:26]([C:28]2[CH:33]=[CH:32][C:31]3[NH:34][C:19]([C:7]4[C:6]5[C:10](=[CH:11][CH:12]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=5)[N:9]([CH:13]5[CH2:18][CH2:17][CH2:16][CH2:15][O:14]5)[N:8]=4)=[N:35][C:30]=3[CH:29]=2)[CH2:27]1
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

7

反応物 3

HCID 23665763Sodium BisulfiteHCID 683850274-(2-Methylmorpholino)benzene-1,2-diamineHCID 866732115-nitro-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole-3-carbaldehyde

生成物 1

HCID 178429876HCID 178429876、化合物収率 55.5%

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid触媒
HCID 8028
Tetrahydrofuran
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
70 °C

実験手順

5-Nitro-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole-3-carbaldehyde (150 mg, 0.545 mmol) and 4-(2-methylmorpholino)benzene-1,2-diamine (113 mg, 0.545 mmol) were dissolved in THF (10 mL) and 2N HCl (1 drop) was added. The solution was heated at a gentle reflux for 30 min. Then, 1N sodium bisulfite (104 mg, 1 mmol; 2 mL of a 1N solution) was added and heated at reflux (70° C.) overnight. The solution was cooled to room temperature, and diluted with ethyl acetate (40 mL). The mixture was washed with water and brine, dried over Na2SO4, and concentrated. Purification by flash chromatography (5% CH3OH/CH2Cl2) afforded the title compound (140 mg). 1H NMR: (400 MHz, CDCl3): δ 9.56 (d, 1H, J=1.6 Hz), 8.28 (m, 1H), 7.74 (d, 1H, J=8.8 Hz), 7.64 (m, 1H), 7.36 (m, 1H), 7.03-6.96 (m, 1H), 5.75 (dd, 1H, J=2.8 and 6.4 Hz), 3.99 (m, 2H), 3.79 (m, 3H), 3.38 (m, 2H), 2.84 (m, 1H), 2.51 (m, 2H), 2.11 (m, 2H), 1.86 (m, 1H), 1.74 (m, 2H), 1.22 (d, 3H, J=6.4 Hz).

後処理

  1. temperatureThe solution was heated at
  2. temperaturea gentle reflux for 30 min
  3. temperatureheated
  4. temperatureThe solution was cooled to room temperature
  5. washThe mixture was washed with water and brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated
  8. customPurification by flash chromatography (5% CH3OH/CH2Cl2)

出典と根拠

ORDレコード
ord-328a7e4ea1074e7eb8da8750dcb862c4
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08569511B2

反応ノート

読み込み中…

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