Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → 1,3-dihydro-1-(3-hydroxypropyl)-5-methyl-2H-benzimidazol-2-one methanesulfonate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | 1,3-dihydro-1-(3-hydroxypropyl)-5-methyl-2H-benzimidazol-2-one | HCID 20385582 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 1,3-dihydro-1-(3-hydroxypropyl)-5-methyl-2H-benzimidazol-2-one methanesulfonate | HCID 86735356 | 58% |
반응 단계
To a stirred solution of 18.5 parts of 1,3-dihydro-1-(3-hydroxypropyl)-5-methyl-2H-benzimidazol-2-one in 325 parts of dichloromethane are added 11.9 parts of N,N-diethylethanamine. Then there are added dropwise (slowly) 11.5 parts of methanesulfonyl chloride. Upon completion, stirring is continued for 1 hour at reflux temperature. After cooling, the reaction mixture is washed with water, dried, filtered and evaporated. The solid residue is crystallized from 4-methyl-2-pentanone, yielding 15 parts (58%) of 1,3-dihydro-1-(3-hydroxypropyl)-5-methyl-2H-benzimidazol-2-one methanesulfonate; mp. 125° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04126687 |
| 출처 데이터셋 | uspto-grants-1978_11 |
| ORD ID | ord-f9532ad887d84cd2936f068e62980db9 |
| 출처 메모 | uspto-grants-1978_11 |