Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Benzenesulfonic acid, 3-amino-5-chloro-4-methyl- → N5-(3-chloro-2-methyl-5-sulfophenyl)-L-glutamine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Benzenesulfonic acid, 3-amino-5-chloro-4-methyl- | HCID 80806 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | HOAt | HCID 181649 | — |
| 반응물 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 반응물 | Boc-Glu-OtBu hydrochloride | HCID 131731743 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Trifluoroacetic acid | HCID 6422 | — |
| 용매 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 생성물 | N5-(3-chloro-2-methyl-5-sulfophenyl)-L-glutamine | HCID 45275582 | — |
반응 단계
After 2 ml of DMF and 0.52 ml (3 mmol) of DIEA were added to 303 mg (1 mmol) of Boc-Glu-OtBu hydrochloride, 221 mg (1 mmol) of 3-amino-5-chloro-4-methylbenzenesulfonic acid, 160 mg (1.3 mmol) of HOAt and 410 mg (1.3 mmol) of HATU, the mixture was stirred at room temperature overnight. The reaction solution was diluted in water-acetonitrile and purified in accordance with the purification step A to give the protected form of the product. The protected product obtained was dissolved in 5 ml of trifluoroacetic acid and stirred for 2 hours. After the solvent was removed by distillation, the mixture was purified in accordance with the purification step A to give the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08877739B2 |
| 출처 데이터셋 | uspto-grants-2014_11 |
| ORD ID | ord-514188b64829444189e1edd87a4f6c62 |
| 출처 메모 | uspto-grants-2014_11 |