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

HRID 1095473

反応式

HRID 1095473 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 HCl. After refluxed for 16 h, the reaction mixture was cooled and water (20 mL) was added. The precipitated was filtered and washed thoroughly with water and hexanes to give 3,4,5,6,7,8-hexahydrobenzo[4,5]thieno[2,3-d]pyrimidin-4-one (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 precipitated was filtered
  4. washwashed thoroughly with water and hexanes

出典と根拠

ORDレコード
ord-51f1f703728b47d49289891ecd01cd75
出典データセット
uspto-grants-2012_03
特許番号
US08138194B2

関連ノート

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