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

HRID 33403

反応式

HRID 33403 の反応式
[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

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 16916Chloromethyl methyl sulfideHCID 9943277HCID 9943277、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-80b11ab93b1b40e5adca360a41e3dbd5
出典データセット
uspto-grants-2008_09
特許番号
US07429598B2

関連ノート

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