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Calcium Carbonate → 3-Chloropropyl (4-hydroxy-2-nitrophenyl)carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Calcium Carbonate | HCID 10112 | — |
| 反応物 | Carbonochloridic acid, 3-chloropropyl ester | HCID 69399 | — |
| 反応物 | 4-Amino-3-Nitrophenol | HCID 3758882 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 3-Chloropropyl (4-hydroxy-2-nitrophenyl)carbamate | HCID 20244590 | — |
反応手順
77 g (0.5 mole) of 3-nitro-4-aminophenol are dissolved in 200 ml of dimethoxy ethane, 27 g of calcium carbonate are added, and 80 g (0.51 mole) of γ-chloropropyl chloroformate are added dropwise at 70° C. After 1 hour, the reaction mixture is filtered hot and the filtrate is stirred into 700 ml of ice-water, after which 128 g (93%) of the desired compound precipitate. The melting point is 103°-105° C., and after recrystallisation from toluene is 106° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04575378 |
| 出典データセット | uspto-grants-1986_03 |
| ORD ID | ord-f7719ddf30034dadbe3f7e7ec4fec665 |
| 出典メモ | uspto-grants-1986_03 |