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Dichloromethane → Ammonium Hydroxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 2-chloro-N-(2,4-dihydroxyphenyl)acetamide | HCID 52904873 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Ammonium Hydroxide | HCID 14923 | — |
| 生成物 | 7-hydroxy-3,4-dihydro-2H-1,4-benzoxazin-3-one | HCID 10057870 | — |
反応手順
To a solution of 2-chloro-N-(2,4-dihydroxyphenyl)acetamide (20 g, 0.0995 mol) in CH2Cl2 (250 mL) sodium hydride (7.164 g, 0.2985 mol) was slowly added at RT. The resulting mixture was stirred for 6 h before water (10 mL) was slowly added. The solution was concentrated in vacuo and purified with column chromatography using 100% CH2Cl2→25%→40% 90:10:1 CH2Cl2:MeOH:NH4OH to yield the title compound. MS (ESI, pos. ion) m/z: 166 (M+1). Mass cal'd for C8H7NO3: 165.04.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08178557B2 |
| 出典データセット | uspto-grants-2012_05 |
| ORD ID | ord-ba0db010d25645a4b1a030b8f4409f51 |
| 出典メモ | uspto-grants-2012_05 |