참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Formaldehyde | HCID 712 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 1,4-Butanediol | HCID 8064 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 2-Methyl-1,4-butanediol | HCID 18053 | — |
| 반응물 | 2,3-Dihydrofuran | HCID 70934 | — |
| 반응물 | Tetrahydro-2-hydroxyfuran | HCID 93002 | — |
| 반응물 | 4-Hydroxybutanal | HCID 93093 | — |
| 반응물 | HCID 178418361 | HCID 178418361 | — |
| 촉매 | Nickel | HCID 935 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4-Hydroxybutyraldehyde 2-hydroxytetrahydrofuran | HCID 86743497 | — |
반응 단계
The 4-hydroxybutyraldehyde/2-hydroxytetrahydrofuran was prepared by adding 20 parts of 2,3-dihydrofuran to 10 parts of 2% H2SO4 over about 20 minutes, keeping the temperature at 35° with cooling. The mixture was then neutralized with 30% NaOH. The organic portion of the resulting homogeneous product was a 2:1 mixture of 4-hydroxybutyraldehyde and its cyclic hemiacetal, 2-hydroxytetrahydrofuran. Thirty parts of that mixture were mixed with 10 parts of water, 4.3 parts of 37% aqueous formaldehyde, 0.53 parts of 30% NaOH, and 2 parts of Raney nickel. Hydrogenation was then carried out at 27,576 kPa (gauge) hydrogen at 150° for 2 hours in a shaker tube. The organic portion of the resulting product consisted mainly of 1,4-butanediol and 2-methyl-1,4-butanediol, in a ratio of 55:45. There were also some unidentified higher boilers.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04879420 |
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| 출처 데이터셋 | uspto-grants-1989_11 |
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| ORD ID | ord-adb34929297e49359d06c1c1b69d311e |
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| 출처 메모 | uspto-grants-1989_11 |
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