참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Chloride | HCID 5234 | — |
| 반응물 | 4-Methoxybenzenesulfonyl chloride | HCID 7401 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | Diacetylene glycol | HCID 94973 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2,4-Hexadiyn-1,6-diol bis(p-methoxybenzene sulfonate) | HCID 18628221 | 93% |
반응 단계
Fifty grams of p-methoxybenzenesulfonyl chloride was reacted, at 15° to 18° C., with 11 grams of 2,4-hexadiyn-1,6-diol in 100 ml tetrahydrofuran, while a solution of 20 grams potassium hydroxide in 180 ml water was added dropwise over a 10 minute period. The resulting exothermic reaction was cooled at 15° to 18° C. with the aid of an ice-water bath. After the addition of the potassium hydroxide solution, the solution was allowed to stir overnight at room temperature. The mixture was then poured into 500 ml cold aqueous sodium chloride solution which resulted in a yellow precipitate. The precipitate was collected by filtration, washed with water and dried. Obtained was 41.6 grams (93% yield of theory) of a yellow brown solid, melting point 120° to 122° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04228126 |
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| 출처 데이터셋 | uspto-grants-1980_10 |
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| ORD ID | ord-e2e002cfcdfe4caa8f00335a0f59b455 |
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| 출처 메모 | uspto-grants-1980_10 |
|---|