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Chlorosulfonic acid → 3-Amino-8-bromo-5,6-dihydrobenzo[f]quinazolin-1(2h)-one-9-sulfonylchloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 反応物 | 3-amino-8-bromo-5,6-dihydrobenzo[f]quinazolin-1(2H)-one | HCID 135838183 | — |
| 生成物 | 3-Amino-8-bromo-5,6-dihydrobenzo[f]quinazolin-1(2h)-one-9-sulfonylchloride | HCID 136120935 | 104.3% |
反応手順
Chlorosulfonic acid(100 g) was added to 3-amino-8-bromo-5,6-dihydrobenzo[f]quinazolin-1(2H)-one(6.20 g, 17.8 mmole) and the solution stirred overnight at room temperature. The reaction mixture was poured over ice, the collected solid washed with water, and dried under high vacuum to give 3-amino-8-bromo-5,6-dihydrobenzo[f]quinazolin-1(2H)-one-9-sulfonyl chloride(7.25 g, 90%). 1H NMR (DMSO-d6, 200 MHz) δ: 2.67-2.75 (m, 2H, Ar CH2), 2.81-2.88 (m, 2H, Ar CH2), 7.43 (s, 1H, Ar), 8.23 (br s, 2H, NH2), 8.91(s, 1H, Ar), 9.90-10.50 (v br s, 1H, NH). Anal Calculated for C12H9BrClN3O3S 1/2 H2O.9/20 H2SO4 : C,32.48; H,2.48; N,9.47; S,10.46. Found: C,32.68; H,2.37; N,9.20; S,10.40.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05663337 |
| 出典データセット | uspto-grants-1997_09 |
| ORD ID | ord-b6ba1cd133f04c6fb647717812dbd1f2 |
| 出典メモ | uspto-grants-1997_09 |