참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Ammonium Hydroxide | HCID 14923 | — |
| 반응물 | Ethyl 2-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate | HCID 78262 | — |
| 반응물 | HCID 135916071 | HCID 135916071 | — |
| 용매 | Dimethyl Sulfone | HCID 6213 | — |
| 생성물 | 2-Amino-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-4(3h)-one | HCID 290197 | 60% |
반응 단계
To a 50 mL flask was added 4 (225 mg, 1 mmol), 9 (452 mg, 4 mmol) in DMSO2 (500 mg) was heated at 150° C. for 2 h. The mixture was cooled to room temperature. 15 mL water was added and ammonium hydroxide was used to neutralize the suspension. The brown solid was obtained by filtration, Washed with water and dried. The solid was dissolved in methanol and silica gel was added A dry silica gel plug obtained after evaporation. The plug was then loaded on the column and washed with 5% methanol in chloroform. The fractions containing the desired product (TLC) were pooled and evaporated to afford 132 mg (60%) of 10 as a white solid: 1H NMR (DMSO-d6) δ 1.71 (m, 4H), 2.60 (m, 2H), 2.72 (m, 2H), 6.38 (s, 2H), 10.72 (s, 1H). Anal. calcd for C10H11N3OS: C, 54.28; H, 5.01; N, 18.99: O, 7.23; S, 14.49. Found: C, 53.45; H, 5.06; N, 18.26; S, 14.02.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07982035B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_07 |
|---|
| ORD ID | ord-8665a481f98345b08eef858ab73d4abe |
|---|
| 출처 메모 | uspto-grants-2011_07 |
|---|