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Hexane → HCID 20539492、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Methoxydiphenylphosphine | HCID 77636 | — |
| 反応物 | 4,6-Dichloro-2-(methylthio)pyrimidine | HCID 80531 | — |
| 溶媒 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 生成物 | HCID 20539492 | HCID 20539492 | — |
反応手順
To a stirred refluxing solution of 5.00 g of 4,6-dichloro-2-methylthiopyrimidine in 150 ml of o-dichlorobenzene under nitrogen was added dropwise 15.00 g of methyl diphenylphosphinite over 35 minutes. The mixture was refluxed for 5.5 hours after the addition was completed and then allowed to cool, at which time it was added to 850 ml of n-hexane. The resulting solid was separated by filtration, washed with n-hexane, and recrystallized from 100 ml of ethanol to give 11.00 g of 4,6-bis(diphenylphosphinyl)-2-methylthiopyrimidine (shown by formula in Claim 8) as white crystals, mp 221°-222° C. Anal. Calcd for C29H24N2O2P2S: C, 66.15; H, 4.59; N, 5.32. Found: C, 65.59; 65.59; H, 4.54, 4.75; N, 5.04, 5.01.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04234729 |
| 出典データセット | uspto-grants-1980_11 |
| ORD ID | ord-dd40434377704e66bcdb9580ce352c92 |
| 出典メモ | uspto-grants-1980_11 |