Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → N-[2-(4-Morpholinyl)ethyl]-1,2-benzisoxazol-3-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 4-(2-Chloroethyl)morpholine | HCID 76727 | — |
| 반응물 | 1,2-Benzoxazol-3-amine | HCID 2779749 | — |
| 반응물 | Dichloromethane methanol | HCID 21226129 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | N-[2-(4-Morpholinyl)ethyl]-1,2-benzisoxazol-3-amine | HCID 15453430 | 38.7% |
반응 단계
To a solution of 3-amino-1,2-benzisoxazole (3.5 g) in N,N-dimethylformamide (DMF) (100 ml) was added sodium hydride (0.8 g) under nitrogen. The reaction was stirred one hour at ambient temperature. A solution of 4-(2-chloroethyl)morpholine (4.0 g) in DMF (50 ml) was added followed by heating to 120° C. for one hour. TLC (5% MeOH/DCM) analysis revealed the absence of starting material. The reaction was quenched with water and extracted with EtOAc. The organic layer was washed with water, dried (MgSO4), and concentrated in vacuo. Flash column chromatography (silica gel) eluting with 1.5-2.5% MeOH/DCM afforded the product (2.5 g), m.p. 79-80° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05925766 |
| 출처 데이터셋 | uspto-grants-1999_07 |
| ORD ID | ord-ee78c7c9ad794163916333dec02bd396 |
| 출처 메모 | uspto-grants-1999_07 |