関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2,2,2-Cryptand | HCID 72801 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | Methanesulfonic acid 3-(4-formylphenoxy)propyl ester | HCID 59236855 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 4-(3-Fluoropropoxy)benzaldehyde | HCID 2782971 | — |
反応手順
Potassium fluoride (Fluka, 7.2 mg, 0.124 mmol) and kryptofix 222 (Fluka, 46.7 mg, 0.124 mmol) were dissolved in dry acetonitrile (2.5 ml). After 10 min the mixture was added to a stirred solution of methanesulfonic acid 3-(4-formylphenoxy)propyl ester 13 (16.0 mg, 0.062 mmol) in dry acetonitrile (1.5 ml). The reaction mixture was heated at 60° C. for 30 minutes. The product was confirmed by analytical HPLC (column Phenomenex Luna C18(2) 3 μm 4.6×50 mm, solvents: A=water/0.1% TFA and B=acetonitrile/0.1% TFA; gradient 10-80% B over 10 min; flow 2.0 ml/min, UV detection at 214 and 254 nm) co-eluting with commercial standard (Fluorochem) at 5.0 minutes.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08197793B2 |
|---|
| 出典データセット | uspto-grants-2012_06 |
|---|
| ORD ID | ord-6799a10eada64d6688f75700a3445624 |
|---|
| 出典メモ | uspto-grants-2012_06 |
|---|