참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 5-Benzylidenehydantoin | HCID 97857 | — |
| 반응물 | 5-[[3-Methoxy-2-(phenylmethoxy)phenyl]methylene]-2,4-imidazolidinedione | HCID 54251091 | — |
| 촉매 | Zinc | HCID 23994 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | (RS)-5-[[3-Methoxy-2-(phenylmethoxy)phenyl]methyl]-2,4-imidazolidinedione | HCID 15296728 | 47.1% |
반응 단계
Zinc powder (40.00 g; 0.61 mole) is added to a stirred suspension of 48.00 g (0.16 mole) of the benzylidine hydantoin from Example 3 in 1,200 mL of methanol under nitrogen. Concentrated hydrochloric acid (30 mL) is added and the mixture is heated on the steam bath for 20 minutes (after 10 minutes the starting benzylidene hydantoin dissolves). Another 30 mL of concentrated hydrochloric acid is added and the mixture is heated at reflux for another 20 minutes. The cooled (50° C.) mixture is cautiously filtered and the cake washed with 100 mL of methanol. Water (500 mL) is added to the filtrate to yield 24.60 g of crystalline product; mp 202°-204° C. Recrystallization from methanol gives pure product; mp 205°-207° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05246943 |
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| 출처 데이터셋 | uspto-grants-1993_09 |
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| ORD ID | ord-3b6e898593fa40f990872efa8f46e0d5 |
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| 출처 메모 | uspto-grants-1993_09 |
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