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3-Methoxypropylamine → 2-{4-[N-(3-Methoxypropyl)sulphamoyl]anilino}-4-(1-methylimidazol-5-yl)pyrimidine

HRID 1064310
ノート
印刷プレビュー

反応式

HRID 1064310 の反応式
Cl[S:2]([OH:5])(=O)=[O:3].[NH:6]([C:13]1[N:18]=[C:17]([C:19]2[N:23]([CH3:24])[CH:22]=[N:21][CH:20]=2)[CH:16]=[CH:15][N:14]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C(N(C(C)C)CC)(C)C.[CH3:34][O:35][CH2:36][CH2:37][CH2:38][NH2:39]>S(Cl)(Cl)=O.CCOC(C)=O>[CH3:34][O:35][CH2:36][CH2:37][CH2:38][NH:39][S:2]([C:10]1[CH:11]=[CH:12][C:7]([NH:6][C:13]2[N:18]=[C:17]([C:19]3[N:23]([CH3:24])[CH:22]=[N:21][CH:20]=3)[CH:16]=[CH:15][N:14]=2)=[CH:8][CH:9]=1)(=[O:5])=[O:3]
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 4

HCID 16723-MethoxypropylamineHCID 24638Chlorosulfonic acidHCID 81531DiisopropylethylamineHCID 222734872-Anilino-4-(1-methylimidazol-5-yl)pyrimidine

生成物 1

HCID 222734712-{4-[N-(3-Methoxypropyl)sulphamoyl]anilino}-4-(1-methylimidazol-5-yl)pyrimidine収率 28%

試薬・触媒・溶媒 2

HCID 8857
Ethyl Acetate
溶媒
HCID 24386Thionyl Chloride溶媒

反応条件

温度
0 °C

実験手順

Chlorosulphonic acid (0.22 ml, 3.18 mmol) was added to suspension of 2-anilino-4-(1-methylimidazol-5-yl)pyrimidine (Example 14; 200 mg, 0.80 mmol) in thionyl chloride (4 ml) cooled at 0° C. The mixture was allowed to warm to ambient temperature, stirred for 15 minutes then heated at reflux for 20 minutes. The volatiles were removed by evaporation and the solid residue dried under high vacuum. The residue was suspended in pyridine (3 ml), cooled to −20° C. and diisopropylethyl amine (0.56 ml, 3.98 mmol) followed by 3-methoxypropyl amine (0.16 ml, 1.60 mmol) was added. The reaction mixture was allowed to warm to ambient temperature and stirred for 30 minutes. EtOAc (15 ml) was added and the mixture washed with saturated aqueous sodium hydrogen carbonate solution (15 ml) and then brine (15 ml). The solvent was removed by evaporation and the residue purified by column chromatography eluting with DCM and 2M methanolic ammonia solution (100:0 increasing in polarity to 85:15) to give the title compound 89 mg, (28%) as a solid product. NMR: 1.75 (m, 2H), 2.76 (q, 2H), 3.14 (s, 3H), 3.22-3.30 (m, 2H), 4.01 (s, 3H), 7.25 (d, 1H), 7.34 (t, 1H), 7.70 (d, 2H), 7.77 (s, 1H), 7.83 (s, 1H), 7.91 (d, 2H), 8.47 (d, 1H), 9.92 (s, 1H); m/z 4.03.

後処理

  1. temperatureto warm to ambient temperature
  2. temperaturethen heated
  3. temperatureat reflux for 20 minutes
  4. customThe volatiles were removed by evaporation
  5. customthe solid residue dried under high vacuum
  6. temperaturecooled to −20° C.
  7. additionwas added
  8. temperatureto warm to ambient temperature
  9. stirringstirred for 30 minutes
  10. washthe mixture washed with saturated aqueous sodium hydrogen carbonate solution (15 ml)
  11. customThe solvent was removed by evaporation
  12. customthe residue purified by column chromatography
  13. washeluting with DCM and 2M methanolic ammonia solution (100:0 increasing in polarity to 85:15)

出典と根拠

ORDレコード
ord-400fa12edcd74554a41edca714ca05cf
出典データセット
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06969714B2

反応ノート

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