Formamide → 1,5,6,7-Tetrahydro-4H-cyclopenta(4,5)thieno(2,3-d)pyrimidin-4-one

HRID 22785ノート

反応式

HRID 22785 の反応式
[NH2:1][C:2]1[S:6][C:5]2[CH2:7][CH2:8][CH2:9][C:4]=2[C:3]=1[C:10]([O:12]CC)=O.O.[CH:16]([NH2:18])=O>>[N:1]1[C:2]2[S:6][C:5]3[CH2:7][CH2:8][CH2:9][C:4]=3[C:3]=2[C:10](=[O:12])[NH:18][CH:16]=1

参加物

4

実験手順

A suspension of 11.37 g ethyl 2-amino-5,6-dihydro-4H-cyclopenta[b]thiophene-3-carboxylate in 40 mL formamide was heated for 4 h to 190° C. using a heating mantle, then cooled and poured into 400 mL water. The mixture was then filtered to remove the solid product. The solids were washed successively with 30 mL EtOAc and 200 mL diethyl ether, air dried overnight, then vacuum oven dried for 3 h. The material was used in the subsequent reactions without further purification.

後処理

  1. temperaturewas heated for 4 h to 190° C.
  2. temperaturecooled
  3. filtrationThe mixture was then filtered
  4. customto remove the solid product
  5. washThe solids were washed successively with 30 mL EtOAc and 200 mL diethyl ether, air
  6. customdried overnight
  7. customvacuum oven dried for 3 h
  8. customThe material was used in the subsequent reactions without further purification

出典と根拠

ORDレコード
ord-7015bc9ba75548c697063adb8e79b4d9
出典データセット
uspto-grants-2005_02
特許番号
US06849638B2

反応ノート

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