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2,3-Dimethyl-2-butene → Dimethyl 2,2,3,3-tetramethylcyclopropanedicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,3-Dimethyl-2-butene | HCID 11250 | — |
| 反応物 | 2-Diazonio-1,3-dimethoxy-3-oxoprop-1-en-1-olate | HCID 547673 | — |
| 触媒 | Mercury | HCID 23931 | — |
| 生成物 | Dimethyl 2,2,3,3-tetramethylcyclopropanedicarboxylate | HCID 13415962 | 30.8% |
反応手順
A mixture of 20.0 grams (0.13 mole) of dimethyl diazomalonate and 164.35 grams (1.95 moles) of 2,3-dimethyl-2-butene was photolyzed at room temperature for a period of approximately 47 hours in the presence of a 100-watt Hanovia mercury lamp. Most of the unreacted 2,3-dimethyl-2-butene was removed by distillation, at atmospheric pressure, to a head temperature of 73° C. and the still residue was subjected to flash chromatography on a silica gel column to give 9.00 grams (0.04 mole) of dimethyl 2,2,3,3-tetramethylcyclopropanedicarboxylate. NMR analysis of the product indicated the following:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05292937 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-00b6f8f1372f4d36a710da393e7c716f |
| 出典メモ | uspto-grants-1994_03 |