Hydrochloric Acid → 3-(3,4-dimethoxybenzyl)-6-(1-hydroxyethyl)-1-(tetrahydro-2H-pyran-4-yl)quinazoline-2,4(1H,3H)-dione

HRID 1022495노트

반응식

HRID 1022495 반응식
[C:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[N:10]([CH:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1)[C:9](=[O:20])[N:8]([CH2:21][C:22]1[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[C:24]([O:30][CH3:31])[CH:23]=1)[C:7]2=[O:32])(=[O:3])[CH3:2].[BH4-].[Na+].O.Cl>CO>[CH3:31][O:30][C:24]1[CH:23]=[C:22]([CH:27]=[CH:26][C:25]=1[O:28][CH3:29])[CH2:21][N:8]1[C:7](=[O:32])[C:6]2[C:11](=[CH:12][CH:13]=[C:4]([CH:1]([OH:3])[CH3:2])[CH:5]=2)[N:10]([CH:14]2[CH2:15][CH2:16][O:17][CH2:18][CH2:19]2)[C:9]1=[O:20]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 4311764Sodium borohydrideHCID 497644036-acetyl-3-(3,4-dimethoxybenzyl)-1-(tetrahydro-2H-pyran-4-yl)-quinazoline-2,4(1H,3H)-dione

생성물 1

HCID 497644053-(3,4-dimethoxybenzyl)-6-(1-hydroxyethyl)-1-(tetrahydro-2H-pyran-4-yl)quinazoline-2,4(1H,3H)-dione

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 0.154 of the compound obtained in Step 7.1 and 0.026 g of NaBH4 in 30 ml of MeOH is stirred for 2 hours at room temperature. Water is added and the mixture is neutralized with 1N HCl. The resulting mixture is evaporated under reduced pressure and the residue is taken up in DCM. This solution is filtered and evaporated under reduced pressure. The residue is chromatographed on silica gel, eluting with EtOAc to give 0.14 g of the expected product.

후처리

  1. customThe resulting mixture is evaporated under reduced pressure
  2. filtrationThis solution is filtered
  3. customevaporated under reduced pressure
  4. customThe residue is chromatographed on silica gel
  5. washeluting with EtOAc

출처 및 근거

ORD 기록
ord-9c29573cd38c4e8592c0f2af56a76e16
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722659B2

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