Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tripropylamine → 2-(2-fluorophenyl)-8,9,10,11-tetrahydro[1]benzothieno[3,2-e][1,2,4]triazolo[1,5-c]pyrimidin-5(6H)one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tripropylamine | HCID 7616 | — |
| 반응물 | Methyl Carbamate | HCID 11722 | — |
| 반응물 | 2-Amino-4,5,6,7-tetrahydrobenzo(b)thiophene-3-carbonitrile | HCID 78382 | — |
| 반응물 | 2-Fluorobenzhydrazide | HCID 136288 | — |
| 용매 | 2-Methoxyethanol | HCID 8019 | — |
| 생성물 | 2-(2-fluorophenyl)-8,9,10,11-tetrahydro[1]benzothieno[3,2-e][1,2,4]triazolo[1,5-c]pyrimidin-5(6H)one | HCID 136058249 | 50% |
반응 단계
The methyl carbamate of 2-amino-3-cyano-4,5,6,7-tetrahydrobenzo(b)thiophene (7.08 g), 2-fluorobenzhydrazide (4.66 g), 2-methoxyethanol (100 mL) and tri-n-propylamine (3 mL) are refluxed under nitrogen for 19 hours. The mixture is cooled and the precipitate collected. The mother liquor is treated with methanol (100 mL) and refrigerated 24 hours to produce a second crop of solid. The combined material is recrystallized from 2-methoxyethanol and dried 20 hours at 100°/0.01 mm to afford 2-(2-fluorophenyl)-8,9,10,11-tetrahydro[1]benzothieno[3,2-e][1,2,4]triazolo[1,5-c]pyrimidin-5(6H)one, which decomposes above 316°. The yield is 50%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04831013 |
| 출처 데이터셋 | uspto-grants-1989_05 |
| ORD ID | ord-757ccbfd48df4a8ba2df6af82126b9a5 |
| 출처 메모 | uspto-grants-1989_05 |