참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Isobutylene | HCID 8255 | — |
| 반응물 | (2S)-3-amino-2-(benzenesulfonamido)propanoic Acid | HCID 10752796 | — |
| 반응물 | Ether hydrochloride | HCID 10953452 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | (S)-3-amino-2-benzenesulfonylamino-propionic acid tert-butyl ester hydrochloride | HCID 22853534 | — |
반응 단계
In a Fischer-Porter tube, a mixture of 22-2 (102 g, 42 mmol) and DME (150 mL) was sequentially treated with H2SO4 (6.4 mL, 0.12 mol), cooled to -78° C., and then condensed isobutylene (75 mL). The cooling bath removed. After 2 h, ice-water (250 mL) was added followed by washing with ether (2×). The aqueous phase was basified with aq 5N NaOH, then saturated with NaCl, followed by extraction with EtOAc (3×). The combined extracts were washed with brine dried (MgSO4), and concentrated to give a white solid. This was dissolved in CHCl3 then treated with 1N HCl/ether (22 mL) then concentrated to give 22-3 as a glossy yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05416099 |
|---|
| 출처 데이터셋 | uspto-grants-1995_05 |
|---|
| ORD ID | ord-b0d0a3512ec748a0a355906b81a46fe3 |
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| 출처 메모 | uspto-grants-1995_05 |
|---|
