Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → 5-(2-Bromoacetylamino)-2,3,4,5-tetrahydro-1-benzoxepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Bromoacetyl bromide | HCID 61147 | — |
| 반응물 | 2,3,4,5-Tetrahydro-1-benzoxepin-5-amine | HCID 15619698 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 5-(2-Bromoacetylamino)-2,3,4,5-tetrahydro-1-benzoxepine | HCID 19694270 | 65% |
반응 단계
To a 5 ml methylene chloride solution of 150 mg of 5-amino-2,3,4,5-tetrahydro-1-benzoxepine (Japanese Unexamined Patent Publication (Kokai) No. 4-178381) and 0.15 ml of triethylamine was added dropwise, under ice cooling, 0.08 ml of bromoacetyl bromide. This was then stirred at room temperature for 1 hour. To the reaction was added 5 ml of a saturated aqueous solution of ammonium chloride, then extraction was performed with methylene chloride. The extract was washed with saturated saline, dried, filtered, then concentrated under reduced pressure to obtain a residue which was then purified by silica gel column chromatography (methylene chloride:methanol=25:1) to obtain the above-referenced compound (8) in an amount of 165 mg (yield of 65%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05723475 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-a457ce1a504046278989f2096f1b01fc |
| 출처 메모 | uspto-grants-1998_03 |