Dimethylamine → HCID 178437759, 화합물

HRID 241076

반응식

HRID 241076 반응식
[CH3:1][NH:2][CH3:3].Cl[CH:5]([C:7]1[N:16]=[C:15]([OH:17])[C:14]2[CH2:13][C:12]([CH3:19])([CH3:18])[CH2:11][CH2:10][C:9]=2[N:8]=1)[CH3:6].ClC(C)C#N>>[CH3:1][N:2]([CH3:3])[CH:5]([C:7]1[N:16]=[C:15]([OH:17])[C:14]2[CH2:13][C:12]([CH3:19])([CH3:18])[CH2:11][CH2:10][C:9]=2[N:8]=1)[CH3:6]

참가 물질

4

반응물 3

HCID 674DimethylamineHCID 5192252-ChloropropionitrileHCID 178456123HCID 178456123, 화합물

생성물 1

HCID 178437759HCID 178437759, 화합물수율 96%

반응 조건

온도
80 °C

실험 절차

To a solution of dimethylamine (2M solution in tetrahydrofuran, 4.0 mL, 8.0 mmol) was added 2-(1-chloroethyl)-6,6-dimethyl-5,6,7,8-tetrahydroquinazolin-4-ol (synthesized according to the method of reagent preparation 18 using 2-chloropropionitrile in step 1) (50 mg, 0.21 mmol) and the reaction mixture was stirred in a sealed tube for 16 hours at 80° C. After cooling to room temperature the reaction mixture was concentrated and the residue was partitioned between brine (50 mL) and ethyl acetate (50 mL). The organic layer was separated and washed with brine (20 mL), dried over sodium sulfate, filtered and concentrated to give 2-[1-(dimethylamino)ethyl]-6,6-dimethyl-5,6,7,8-tetrahydroquinazolin-4-ol (50 mg, 96%). MS (EI) for C14H23N3O: 250 (MH+).

후처리

  1. customsynthesized
  2. temperatureAfter cooling to room temperature the reaction mixture
  3. concentrationwas concentrated
  4. customthe residue was partitioned between brine (50 mL) and ethyl acetate (50 mL)
  5. customThe organic layer was separated
  6. washwashed with brine (20 mL)
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-324e2d1ff11845368ba33ed05f09b953
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648066B2

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