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Triethylamine → 7-methoxy-3,4-dihydro-1H-isoquinoline-2-sulfonyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Sulfuryl chloride | HCID 24648 | — |
| 反応物 | 7-Methoxy-1,2,3,4-tetrahydroisoquinoline hydrochloride | HCID 2752197 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 7-methoxy-3,4-dihydro-1H-isoquinoline-2-sulfonyl chloride | HCID 22665676 | — |
反応手順
To a stirred, precooled solution (-40° C.) of 0.41 mL of sulfuryl chloride in 10 mL of chloroform was added a mixture of 1.0 g of 7-methoxy-1,2,3,4-tetrahydro-isoquinoline-hydrochloride and 2.1 mL of triethylamine in 25 mL of chloroform at −40° C. Stirring was continued at −30° C. for one hour and additionally at 5° C. for one hour. The mixture was poured on ice, the organic layer extracted with cold water, dried (sodium sulfate) and concentrated. The residue was redissolved in diethyl ether and chromatographed on silica gel (isohexane/ethyl acetate=8/2 v/v) yielding 0.62 g of 7-methoxy-3,4-dihydro-1H-isoquinoline-2-sulfonyl chloride as an oil. EI-MS: 261 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06194409B1 |
| 出典データセット | uspto-grants-2001_02 |
| ORD ID | ord-69f30d8b5c3547e7bfd517abec3eec15 |
| 出典メモ | uspto-grants-2001_02 |