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Dibenzylphosphate → Phosphoric acid dibenzyl ester 4-(4-tert-butyl-phenylamino)-7-(3-trifluoromethyl-pyridin-2-yl)-quinazolin-2-ylmethyl ester

HRID 2113613
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HRID 2113613 반응식
Cl[CH2:2][C:3]1[N:12]=[C:11]([NH:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]([CH3:23])([CH3:22])[CH3:21])=[CH:16][CH:15]=2)[C:10]2[C:5](=[CH:6][C:7]([C:24]3[C:29]([C:30]([F:33])([F:32])[F:31])=[CH:28][CH:27]=[CH:26][N:25]=3)=[CH:8][CH:9]=2)[N:4]=1.[CH2:34]([O:41][P:42]([O-:52])([O:44][CH2:45][C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1)=[O:43])[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1>C(#N)C>[C:20]([C:17]1[CH:18]=[CH:19][C:14]([NH:13][C:11]2[C:10]3[C:5](=[CH:6][C:7]([C:24]4[C:29]([C:30]([F:32])([F:31])[F:33])=[CH:28][CH:27]=[CH:26][N:25]=4)=[CH:8][CH:9]=3)[N:4]=[C:3]([CH2:2][O:43][P:42](=[O:52])([O:44][CH2:45][C:46]3[CH:47]=[CH:48][CH:49]=[CH:50][CH:51]=3)[O:41][CH2:34][C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)[N:12]=2)=[CH:15][CH:16]=1)([CH3:23])([CH3:22])[CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4193600DibenzylphosphateHCID 58628208[2-Chloromethyl-7-(3-trifluoromethyl-pyridin-2-yl)-quinazolin-4-yl]-(4-t-butyl-phenyl)-amine

생성물 1

HCID 9987362Phosphoric acid dibenzyl ester 4-(4-tert-butyl-phenylamino)-7-(3-trifluoromethyl-pyridin-2-yl)-quinazolin-2-ylmethyl ester

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

Heat a solution of [2-chloromethyl-7-(3-trifluoromethyl-pyridin-2-yl)-quinazolin-4-yl]-(4-t-butyl-phenyl)-amine (417 mg, 0.89 mmol), Ag2O (308 mg, 1.33 mmol), and dibenzylphosphate (370 mg, 1.33 mmol) in acetonitrile at 70° C. for 18 hours. Dilute with additional acetonitrile and filter the hot solution through celite. Concentrate under reduced pressure to give a foam. Crystallize the crude product by dissolving in ether and slowly adding hexanes. Cool the resulting mixture on ice and collect the resulting solid via filtration to afford pure product.

후처리

  1. filtrationfilter the hot solution through celite
  2. concentrationConcentrate under reduced pressure
  3. customto give a foam
  4. customCrystallize the crude product
  5. dissolutionby dissolving in ether
  6. temperatureCool the resulting mixture on ice
  7. customcollect the resulting solid
  8. filtrationvia filtration
  9. customto afford pure product

출처 및 근거

ORD 기록
ord-593f3ae7d5fd4ab79e9f761f318487e0
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07432275B2

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