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Carbon Tetrachloride → (6,7-Diethoxy-quinazolin-4-yl)-(3-ethynyl-phenyl)-amine Hydrochloride

HRID 1288883
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HRID 1288883 반응식
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][C:13]=1[O:14][CH2:15][CH3:16])[N:10]=[CH:9][NH:8][C:7]2=O)[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:38].[C:42]([C:44]1[CH:45]=[C:46]([CH:48]=[CH:49][CH:50]=1)[NH2:47])#[CH:43]>C(O)(C)C>[ClH:38].[CH2:1]([O:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][C:13]=1[O:14][CH2:15][CH3:16])[N:10]=[CH:9][N:8]=[C:7]2[NH:47][C:46]1[CH:48]=[CH:49][CH:50]=[C:44]([C:42]#[CH:43])[CH:45]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 104682Benzenamine, 3-ethynyl-HCID 1354614006,7-diethoxyquinazolin-4(3H)-one

생성물 1

HCID 18925066(6,7-Diethoxy-quinazolin-4-yl)-(3-ethynyl-phenyl)-amine Hydrochloride

시약·촉매·용매 1

HCID 3776
Isopropanol
용매

실험 절차

6,7-Diethoxyquinazolin-4-one (120 mg, 0.512 mmol), triphenylphosphine (295 mg, 1.126 mmol) and 3 mL of carbon tetrachloride were refluxed for 16 hours. The reaction mixture was concentrated in vacuo to a residue which was diluted with 3 mL of isopropyl alcohol and 3-ethynylaniline (66 mg, 0.563 mmol) and refluxed for 3 hours. The cooled reaction mixture was filtered to afford solid title product which was washed with 10 mL of isopropyl alcohol and dried in vacuo at 70° C., 140 mg (75%); mp 269°-270° C.

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo to a residue which
  2. temperaturerefluxed for 3 hours
  3. customThe cooled reaction mixture
  4. filtrationwas filtered

출처 및 근거

ORD 기록
ord-f1f00b96ab6c41558d9684075686e08d
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05747498

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