참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,2-Ethanedithiol | HCID 10902 | — |
| 반응물 | Sodium borohydride | HCID 4311764 | — |
| 반응물 | Methyl 3-chloro-4-cyano-2-methylbenzoate | HCID 68579417 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-Chloro-4-(hydroxymethyl)-3-methylbenzonitrile | HCID 68577571 | 66.5% |
반응 단계
To a pressure reaction flask containing compound 7A (1.5 g, 7.2 mmol) in THF (30 mL) were added 1,2-ethanedithiol (2.4 g, 28.6 mmol) and NaBH4 (812 mg, 21.5 mmol). It was sealed, and heated at 70° C. for 2 hr, and cooled to RT. The reaction mixture was concentrated, dissolved in EtOAc, washed with water, dried over Na2SO4, and concentrated. Recrystallization in EtOAc/hexanes give the title compound (870 mg). (ES) m/z 182 [M+H]+; 204 [M+Na]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07696241B2 |
|---|
| 출처 데이터셋 | uspto-grants-2010_04 |
|---|
| ORD ID | ord-6f973348b7b245bc91aa790a6ac3c759 |
|---|
| 출처 메모 | uspto-grants-2010_04 |
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