참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | 1-Butanone, 1-(4-aminophenyl)- | HCID 15527 | — |
| 반응물 | 3-Thiophenecarboxaldehyde | HCID 68135 | — |
| 용매 | Dimethylacetamide | HCID 31374 | — |
| 용매 | Dichloromethane methanol | HCID 21226129 | — |
| 생성물 | 1-{4-[(Thiophen-3-ylmethyl)amino]phenyl}-butan-1-one | HCID 25127150 | — |
반응 단계
In a 20 mL vial, to a solution of 1-(4-aminophenyl)-butan-1-one (19.64 mg, 0.1 mmol) in DCM/MeOH (0.7 mL) was added a solution of thiophene-3-carbaldehyde (22.4 mg, 0.2 mmol) in DMA (0.8 mL). A solution of acetic acid (18 mg, 0.3 mmol) in DCM/MeOH (0.7 mL) was added, followed by the addition of 160 mg of MP-CNBH3 resin (3 eq.; subst. 2.25 mmoles/g). The vial was capped and was then heated with shaking overnight at 55° C. The progress of the reaction was monitored by LC/MS. After completion of the reaction, the reaction mixture was concentrated to dryness. The residue was dissolved in 1:1 DMSO/MeOH. Purification by reverse phase HPLC (TFA method) gave the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09242933B2 |
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| 출처 데이터셋 | uspto-grants-2016_01 |
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| ORD ID | ord-e90a9289aeec45d7859d29bd7bf3c7e6 |
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| 출처 메모 | uspto-grants-2016_01 |
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