Potassium Carbonate → 8'-chloro-5'-([methylthio]methoxy)-1'H-spiro[cyclohexane-1,4'-quinazolin]-2'(3'H)-one

HRID 33403

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HRID 33403 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([OH:18])=[C:6]2[C:11]=1[NH:10][C:9](=[O:12])[NH:8][C:7]12[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1.C(=O)([O-])[O-].[K+].[K+].[CH3:25][S:26][CH2:27]Cl>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:18][CH2:25][S:26][CH3:27])=[C:6]2[C:11]=1[NH:10][C:9](=[O:12])[NH:8][C:7]12[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 16916Chloromethyl methyl sulfideHCID 9943277HCID 9943277, 화합물

생성물 1

HCID 129855038'-chloro-5'-([methylthio]methoxy)-1'H-spiro[cyclohexane-1,4'-quinazolin]-2'(3'H)-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

To a solution of 8′-chloro-5′-hydroxy-1′H-spiro[cyclohexane-1,4′-quinazolin]-2′(3′H)-one, which can be prepared according to processes disclosed in example 63 of PCT/EP02/03594 (6 g, 2.25 mmol) in dimethylformamide (6 mL) was added potassium carbonate (0.776 g, 5.6 mmol) and chloromethyl methyl sulfide (0.26 mL, 2.7 mmol). The mixture was stirred in a sealed tube at 100° C. for 3 days. Dimethylformamide was removed by evaporation in vacuo. Water was added to the residue and the aqueous layer was extracted twice with ethyl acetate.

후처리

  1. customDimethylformamide was removed by evaporation in vacuo
  2. additionWater was added to the residue
  3. extractionthe aqueous layer was extracted twice with ethyl acetate

출처 및 근거

ORD 기록
ord-80b11ab93b1b40e5adca360a41e3dbd5
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429598B2

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