Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 2,4-Dimethoxybenzylamine | HCID 597250 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | HCID 20784931 | HCID 20784931 | — |
| Product | HCID 20784932 | HCID 20784932 | — |
Reaction Steps
A stirred solution of 4-[(2,4-dimethoxy-benzylamino)-methyl]-1-(tetrahydro-pyran-2-yl)-1H-pyrazole-3-carboxylic acid ethyl ester [1 g, Reference Example 54(b)] in tetrahydrofuran (25 ml) was treated with 2,4-dimethyoxybenzylamine (0.596 ml). After stirring for 12 hours sodium triacetoxyborohydride (1.68 g) was added to the reaction mixture and the reaction mixture was stirred for a further 1 hour before partitioning between ethyl acetate (200 ml) and saturated sodium hydrogencarbonate (200 ml). The aqueous layer was extracted twice with ethyl acetate (100 ml) and the combined organic layers were dried over magnesium sulfate and then concentrated in vacuo to yield 4-{[(2,4-dimethoxy-benzyl)-(morpholine-4-carbonyl)-amino]-methyl}-1-(tetrahydro-pyran-2-yl)-1H-pyrazole-3-carboxylic acid ethyl ester (1.66 g) as a yellow oil. LC-MS (Method B): RT=2.27 minutes, 404.17 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08288425B2 |
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| Source dataset | uspto-grants-2012_10 |
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| ORD ID | ord-105925269f1e4442bb713899839c4143 |
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| Source note | uspto-grants-2012_10 |
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