関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | HCID 178446411 | HCID 178446411 | — |
| 触媒 | HCID 178479819 | HCID 178479819 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | HCID 178435146 | HCID 178435146 | — |
反応手順
The intermediate (114 mg, 0.140 mmol) from Step 4(B) was dissolved in 45 mL of 1,2-dichloroethane, followed by the addition of Grubbs Catalyst 1st Generation (22 mg, 0.020 mmol) with 1 mL of 1,2-dichloroethane. The resulted reaction mixture was stirred at 70° C. for 6 hrs. (additional 14 mg of Grubbs Catalyst was added 2 hrs. after the initial addition) Solvent was evaporated in vacuo to give a crude product, which was purified by flash chromatography (10% EtOAc/DCM, Rf 0.19) to give 75 mg (68%, theoretical yield 110 mg) of the product, which is a mixture of cis and trans isomers. LCMS (method B) RT 3.78 min., MH+787.8.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07732434B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-d76a862a56524df588a1981e5e8506c5 |
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| 出典メモ | uspto-grants-2010_06 |
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