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Hydrazine, propyl- → 2,3,3a,4,6,7-Hexahydro-3-phenyl-7-(phenylmethylene)-2-propylthiopyrano[4,3-c]pyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine, propyl- | HCID 42007 | — |
| 反応物 | tetrahydro-3,5-bis(phenylmethylene)-4H-thiopyran-4-one | HCID 336779 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2,3,3a,4,6,7-Hexahydro-3-phenyl-7-(phenylmethylene)-2-propylthiopyrano[4,3-c]pyrazole | HCID 53974971 | 57.5% |
反応手順
A mixture of 5.84g of tetrahydro-3,5-bis-(phenylmethylene)-4H-thiopyran-4-one and 1.48g of n-propyl hydrazine in 100ml of methanol is heated at reflux temperature for 3 hours. Upon cooling, solids are collected and washed with methanol. Recrystallization from methanol gives 4.0g of material, melting point 111°-120°C. Two recrystallizations from acetonitrile yield 2.0g of the title compound, melting point 119.5°-122°C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03979381 |
| 出典データセット | uspto-grants-1976_09 |
| ORD ID | ord-d7486b977a2c4d8a9645820d2dc0b725 |
| 出典メモ | uspto-grants-1976_09 |