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Dimethylamine → HCID 178487757, 화합물

HRID 241035
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HRID 241035 반응식
[CH3:1][NH:2][CH3:3].Cl.Cl[CH2:6][C:7]1[N:16]=[C:15]([OH:17])[C:14]2[C:9](=[CH:10][C:11]([O:18][CH3:19])=[CH:12][CH:13]=2)[N:8]=1>>[CH3:1][N:2]([CH2:6][C:7]1[N:16]=[C:15]([OH:17])[C:14]2[C:9](=[CH:10][C:11]([O:18][CH3:19])=[CH:12][CH:13]=2)[N:8]=1)[CH3:3]
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참가 물질

3

반응물 2

HCID 674DimethylamineHCID 178487747HCID 178487747, 화합물

생성물 1

HCID 178487757HCID 178487757, 화합물수율 97.6%

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온도
50 °C

실험 절차

To a solution of dimethylamine (2M solution in tetrahydrofuran, 40.0 mL, 80.0 mmol) was added 2-(chloromethyl)-7-(methyloxy)quinazolin-4-ol hydrochloride (7.5 g, 29 mmol) and the reaction mixture was stirred for 90 minutes at 50° C. After cooling it to room temperature the reaction mixture was concentrated and the residue was partitioned between water (100 mL) and ethyl acetate (250 mL). The organic layer was separated and washed with water (100 mL), saturated sodium bicarbonate (100 mL) and brine (100 mL), dried over sodium sulfate, filtered and concentrated to give 2-[(dimethylamino)methyl]-7-(methyloxy)quinazolin-4-ol (6.6 g, 97%). MS (EI) for C12H15N3O2: 234 (MH+).

후처리

  1. temperatureAfter cooling it to room temperature the reaction mixture
  2. concentrationwas concentrated
  3. customthe residue was partitioned between water (100 mL) and ethyl acetate (250 mL)
  4. customThe organic layer was separated
  5. washwashed with water (100 mL), saturated sodium bicarbonate (100 mL) and brine (100 mL)
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b4cb3f57005e4f08a7cd19e0fe3f6e52
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08648066B2

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