tert-Butanol → HCID 66623412, 화합물

HRID 415019노트

반응식

HRID 415019 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH2:16])[CH:5]=[CH:6][C:7]=1[O:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=1.Cl[C:18]1[C:27]2[C:22](=[CH:23][C:24]([O:32][CH3:33])=[C:25]([O:28]C(=O)C)[CH:26]=2)[N:21]=[CH:20][N:19]=1.CC(O)(C)C>ClCCCl>[Cl:1][C:2]1[CH:3]=[C:4]([NH:16][C:18]2[C:27]3[C:22](=[CH:23][C:24]([O:32][CH3:33])=[C:25]([OH:28])[CH:26]=3)[N:21]=[CH:20][N:19]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=1

참가 물질

5

반응물 3

HCID 6386tert-ButanolHCID 167812123-Chloro-4-(2-pyridylmethoxy)anilineHCID 220221604-Chloro-7-methoxyquinazolin-6-yl acetate

생성물 1

HCID 66623412HCID 66623412, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

3-Chloro-4-(pyridin-2-ylmethoxy)-phenylamine (3.9 g, 16.62 mmol) and acetic acid 4-chloro-7-methoxy-quinazolin-6-yl ester (4.62 g, 18.28 mmol) were dissolved in a 1:1 mixture of DCE:t-BuOH (50 mL). The reaction mixture was refluxed for 19 hours and then cooled to room temp. Solvent was removed via rotovap. The crude residue was then suspended in MeOH (80 mL) and NH4OH (8 mL, 30% in water) was added to the mixture. Stir for 15 hours at room temp. The reaction was heated to 100° C. and stirred for 1 hour. Cool to 0° C. and product was isolated by filtration and washed with cold MeOH to give 5 g (12.2 mmol, 67% over two steps) of desired product.

후처리

  1. temperatureThe reaction mixture was refluxed for 19 hours
  2. customSolvent was removed via rotovap
  3. additionNH4OH (8 mL, 30% in water) was added to the mixture
  4. temperatureThe reaction was heated to 100° C.
  5. stirringstirred for 1 hour
  6. temperatureCool to 0° C.
  7. customproduct was isolated by filtration
  8. washwashed with cold MeOH

출처 및 근거

ORD 기록
ord-191611df4d16471cb9904eadc4fb60c0
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08088766B2

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