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Methoxydiphenylphosphine → 5-Bromo-4-diphenylphosphinyl-2-methylthiopyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methoxydiphenylphosphine | HCID 77636 | — |
| 反応物 | 5-Bromo-4-chloro-2-(methylsulfanyl)pyrimidine | HCID 265881 | — |
| 溶媒 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 生成物 | 5-Bromo-4-diphenylphosphinyl-2-methylthiopyrimidine | HCID 20539470 | 49.3% |
反応手順
To a stirred, refluxing mixture of 3.56 g of 5-bromo-4-chloro-2-methylthiopyrimidine in 100 ml of o-dichlorobenzene under nitrogen was added dropwise 10.00 g of methyl diphenylphosphinite. After the addition was completed, the mixture was refluxed for 6 hours and then allowed to cool. Volatiles were removed from the mixture under vacuum, and the residue was recrystallized from 30 ml of 1-chlorobutane and dried at 50° C./0.1 mm (13 Pa) to give 2.97 g of 5-bromo-4-diphenylphosphinyl-2-methylthiopyrimidine (shown by formula in Claim 7) as white crystals, mp 124°-127° C. Anal. Calcd for C17H14BrN2OPS: C, 50.39; H, 3.48; N, 6.91. Found: C, 50.54; H, 3.67; N, 6.84.
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-b1dcd8c8a1f44f40af31fe94fd18ce6a |
| 出典メモ | uspto-grants-1980_11 |