참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Dibenzylphosphate | HCID 4193600 | — |
| 반응물 | (2-hydoxy-ethyl)-carbamic acid 3-(1-methyl-1H-indol-3-yl)-4-(1-methyl-6-nitro-1H-indol-3-yl)-2,5-dioxo-2,5-dihydro-pyrrol-1-ylmethyl ester | HCID 9892774 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 131723880 | HCID 131723880 | 54% |
반응 단계
Triphenylphosphine (95 mg, 0.36 mmol) and dibenzyl phosphate (101 mg, 0.36 mmol) were added to a solution of (2-Hydoxy-ethyl)-carbamic acid 3-(1-methyl-1H-indol-3-yl)-4-(1-methyl-6-nitro-1H-indol-3-yl)-2,5-dioxo-2,5-dihydro-pyrrol-1-ylmethyl ester, prepared as in example 19 (150 mg, 0.289 mmol) in THF (6 mL). The mixture was cooled at −78° C. Diethyl azodicarboxiate (0.057 mL, 0.36 mmol) was added dropwise over 5 min. The cooling bath was removed and the mixture was stirred overnight. The mixture was then evaporated. Chromatography of the residue over silica gel using 2:1-4:1 EtOAc/hexanes gave [2-bis-benzyloxy-phosphoryloxy)-ethyl]-carbamic acid 3-(1-methyl-1H-indol-3-yl)-4-(1-methyl-6-nitro-1H-indol-3-yl)-2,5-dioxo-2,5-dihydro-pyrrol-1-ylmethyl ester (121 mg, 54%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06559164B1 |
|---|
| 출처 데이터셋 | uspto-grants-2003_05 |
|---|
| ORD ID | ord-5920eaef75b444e2995e032250df7c23 |
|---|
| 출처 메모 | uspto-grants-2003_05 |
|---|