참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Pentanethiol | HCID 8067 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1-Chloro-3-iodopropane | HCID 81363 | — |
| 반응물 | Sodium | HCID 5360545 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 19023126 | HCID 19023126 | 59% |
반응 단계
A suspension of sodium hydride (4.0 g, 100 mmole) in dry tetrahydrofuran (350 mL) under a nitrogen atmosphere was cooled in an ice bath. Pentyl mercaptan (10.8 g, 100 mmole) was added dropwise over 10 minutes. The resulting suspension of sodium alkylmercaptide was added in portions over 30 minutes to a stirred solution of 1-chloro-3-iodopropane (20.44 g, 100 mmole) in tetrahydrofuran (450 mL) that had been cooled to -78° C. The mixture was allowed to warm to ambient temperature overnight, then washed with brine, dried over MgSO4, and concentrated under vacuum. The resultant oil was distilled under water aspirator pressure to yield the desired product (10.67 g, 59% yield), b.p. 113°-119° C. (20 mm Hg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05292627 |
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| 출처 데이터셋 | uspto-grants-1994_03 |
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| ORD ID | ord-960bbc68ef3c4fda9453a5a236b22609 |
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| 출처 메모 | uspto-grants-1994_03 |
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