Formic Acid → 5,6,7,8-Tetrahydro(1)benzothieno(2,3-D)pyrimidin-4(3H)-one

HRID 1891024

反応式

HRID 1891024 の反応式
[NH2:1][C:2]1[S:6][C:5]2[CH2:7][CH2:8][CH2:9][CH2:10][C:4]=2[C:3]=1[C:11]#[N:12].[CH:13](O)=O.Cl.[OH2:17]>>[N:1]1[C:2]2[S:6][C:5]3[CH2:7][CH2:8][CH2:9][CH2:10][C:4]=3[C:3]=2[C:11](=[O:17])[NH:12][CH:13]=1

参加物

5

反応物 4

HCID 284Formic AcidHCID 313Hydrochloric AcidHCID 962WaterHCID 783822-Amino-4,5,6,7-tetrahydrobenzo(b)thiophene-3-carbonitrile

生成物 1

HCID 986145,6,7,8-Tetrahydro(1)benzothieno(2,3-D)pyrimidin-4(3H)-one収率 77%

実験手順

To a mixture of 2-amino-4,5,6,7-tetrahydrobenzo[b]thiophen-3-yl cyanide (0.9 g) and formic acid (10 mL) was added 0.1 mL conc. HCl. After refluxed for 16 h, the reaction mixture was cooled and water (20 mL) was added. The precipitate was collected by filtration and washed thoroughly with water and hexanes to give the title compound (0.8 g, 77%). 1H NMR (300 MHz, CDCl3): δ 7.91 (s, 1H), 3.03-3.00 (m, 2H), 2.80-2.77 (m, 2H), 1.89-1.83 (m, 4H).

後処理

  1. temperatureAfter refluxed for 16 h
  2. temperaturethe reaction mixture was cooled
  3. filtrationThe precipitate was collected by filtration
  4. washwashed thoroughly with water and hexanes

出典と根拠

ORDレコード
ord-0503b9880e4945daaed7066ffffc3269
出典データセット
uspto-grants-2013_08
特許番号
US08507502B2

関連ノート

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