참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 반응물 | 2,2-dimethyl-3,4-dihydro-2H-benzo[e][1,3]oxazine | HCID 66859222 | — |
| 생성물 | [2-(Propan-2-ylamino)phenyl]methanol | HCID 10797123 | 95% |
반응 단계
A solution of 2,2,-dimethyl-1,4-dihydro-2H-benzo[1,3]oxazine (125 g, 0.77 mol) in THF (1 L) was filtered through a scintillation funnel and then added dropwise via an addition funnel, over a period of 2.5 h, to a stirred solution of 1.0 M LiAlH4 in THF (800 mL) at 0° C. The reaction was quenched by slow portionwise addition of Na2SO4.10H2O (110 g), over a period of 1.5 h, at 0° C. The reaction mixture was stirred overnight, filtered and the solid salts were washed thoroughly with THF. The filtrate was concentrated under reduced pressure to yield 2-isopropylaminophenylmethanol (120 g, 95%) as a yellow oil. 1H NMR (CDCl3; 300 MHz): 1.24 (d, 6H, CH(CH3)2), 3.15 (bs, 1H, OH), 3.61 (sept, 1H, CH(CH3)2), 4.57 (s, 2H, CH2), 6.59 (t, 1H, ArH), 6.65 (d, 1H, ArH), 6.99 (d, 1H, ArH), 7.15 (t, 1H, ArH).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07728006B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-b365b3cf20f740868d5dd9e747f42a18 |
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| 출처 메모 | uspto-grants-2010_06 |
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