Trifluoroacetic acid → HCID 178493836, 화합물

HRID 536215노트

반응식

HRID 536215 반응식
C([O:8][C:9]1[CH:10]=[CH:11][C:12]2[C:13]3[N:14]([CH2:22][CH2:23][N:24]=3)[C:15]([NH2:21])=[N:16][C:17]=2[C:18]=1[O:19][CH3:20])C1C=CC=CC=1.[C:25]([OH:31])([C:27]([F:30])([F:29])[F:28])=[O:26]>CO>[F:28][C:27]([F:30])([F:29])[C:25]([OH:31])=[O:26].[F:28][C:27]([F:30])([F:29])[C:25]([OH:31])=[O:26].[NH2:21][C:15]1[N:14]2[CH2:22][CH2:23][N:24]=[C:13]2[C:12]2[CH:11]=[CH:10][C:9]([OH:8])=[C:18]([O:19][CH3:20])[C:17]=2[N:16]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 1784938207-methoxy-8-phenylmethoxy-2,3-dihydroimidazo[1,2-c]quinazolin-5-amine

생성물 1

HCID 178493836HCID 178493836, 화합물수율 100%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

3-(Benzyloxy)-6-(4,5-dihydro-1H-imidazol-2-yl)-2-methoxyaniline (Step 7, 30 g, 93 mmol) was added portionwise over 1 h to a round bottom flask containing TFA (400 mL) precooled with an ice bath. The reaction mixture was heated to 60° C. and allowed to stir at this temperature for 17 h at which time it was cooled to rt and the reaction mixture concentrated under reduced pressure. The resulting residue was taken up in DCM and hexanes and concentrated under reduced pressure. The material thus obtained was dissolved in MeOH and DCM (250 mL, 1:1) and concentrated under reduced pressure. The resulting solid was dried overnight under vacuum with low heat to give the title compound (100%): 1H NMR (DMSO-d6) δ: 7.61 (1H, m), 6.87 (1H, m), 4.15 (2H, br t), 4.00 (2H, m), 3.64 (3H, s).

후처리

  1. customprecooled with an ice bath
  2. temperaturewas cooled to rt
  3. concentrationthe reaction mixture concentrated under reduced pressure
  4. concentrationhexanes and concentrated under reduced pressure
  5. customThe material thus obtained
  6. concentrationDCM (250 mL, 1:1) and concentrated under reduced pressure
  7. customThe resulting solid was dried overnight under vacuum
  8. temperaturewith low heat

출처 및 근거

ORD 기록
ord-95b3caaf46d14070b18d160e80b9664e
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859572B2

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