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N-{3-[(2,5-dichloropyrimidin-4-yl)amino]benzyl}-3-nitrobenzamide → 3-Amino-N-{3-[(2,5-dichloropyrimidin-4-yl)amino]benzyl}benzamide

HRID 541817
ノート
印刷プレビュー

反応式

HRID 541817 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:10]=[C:11]([CH:25]=[CH:26][CH:27]=2)[CH2:12][NH:13][C:14](=[O:24])[C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([N+:21]([O-])=O)[CH:16]=2)[C:5]([Cl:28])=[CH:4][N:3]=1>O.CO.C(O)(=O)C.[Fe]>[NH2:21][C:17]1[CH:16]=[C:15]([CH:20]=[CH:19][CH:18]=1)[C:14]([NH:13][CH2:12][C:11]1[CH:25]=[CH:26][CH:27]=[C:9]([NH:8][C:6]2[C:5]([Cl:28])=[CH:4][N:3]=[C:2]([Cl:1])[N:7]=2)[CH:10]=1)=[O:24]
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

6

反応物 1

HCID 57961607N-{3-[(2,5-dichloropyrimidin-4-yl)amino]benzyl}-3-nitrobenzamide

生成物 1

HCID 579622043-Amino-N-{3-[(2,5-dichloropyrimidin-4-yl)amino]benzyl}benzamide収率 117.2%

試薬・触媒・溶媒 4

HCID 23925Iron触媒HCID 176Acetic Acid溶媒HCID 887Methanol溶媒
HCID 962
Water
溶媒

反応条件

温度
0 °C

実験手順

To a solution N-{3-[(2,5-dichloropyrimidin-4-yl)amino]benzyl}-3-nitrobenzamide (400.0 mg, 0.956 mmol) in water (0.7 mL), methanol (3.7 mL) and acetic acid (1.5 mL) was added iron (130 mg, 2.4 mmol) powder in small quantities. When the addition was completed, the very cloudy mixture was stirred at 0° C. for 1 h and then heat at 40° C. for 3 h. The mixture was filtered, and the cake was washed with MeOH/EtOAc. The filtrate was concentrated and the residue was diluted with H2O, then the aqueous layer was extracted with EtOAc three times. The combined organic layers were dried, filtered and concentrated to give the desired product as an off-white powder (435 mg). LCMS for C18H15Cl2N5O (M+H)+: m/z=388.0, 390.0, 392.0. 1H NMR (400 MHz, CD3OD): δ 8.20 (s, 1H), 7.59 (t, J=2.0 Hz, 1H), 7.52 (d, J=8.0 Hz, 1H), 7.36 (t, J=8.0 Hz, 1H), 7.24 (m, 2H), 7.20 (m, 2H), 6.93 (m, 1H), 4.60 (s, 2H).

後処理

  1. additionWhen the addition
  2. temperatureheat at 40° C. for 3 h
  3. filtrationThe mixture was filtered
  4. washthe cake was washed with MeOH/EtOAc
  5. concentrationThe filtrate was concentrated
  6. additionthe residue was diluted with H2O
  7. extractionthe aqueous layer was extracted with EtOAc three times
  8. customThe combined organic layers were dried
  9. filtrationfiltered
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-cae36fe49d1644e8bbde3f145f00ce12
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08871753B2

反応ノート

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