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

HRID 22785노트

반응식

HRID 22785 반응식
[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

참가 물질

4

반응물 3

HCID 713FormamideHCID 962WaterHCID 264105ethyl 2-amino-4H,5H,6H-cyclopenta[b]thiophene-3-carboxylate

생성물 1

HCID 2034201,5,6,7-Tetrahydro-4H-cyclopenta(4,5)thieno(2,3-d)pyrimidin-4-one

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7015bc9ba75548c697063adb8e79b4d9
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06849638B2

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