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Cesium carbonate → 2-[5-{2,8-Dimethyl-5H-dibenzo[a,d]cyclohepten-5-yl}-3,4-dihydro-2,4-dioxo-1(2H)-pyrimidinyl]-4-[[[1,1-dimethylethoxy]carbonylmethyl]amino]-5-pyrimidinecarboxylic acid, methyl ester

HRID 1871987
ノート
印刷プレビュー

反応式

HRID 1871987 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[C:5]([C:17]([O:19][CH3:20])=[O:18])=[CH:4][N:3]=1.[CH3:21][C:22]1[CH:45]=[CH:44][C:25]2[CH:26]([C:36]3[C:37](=[O:43])[NH:38][C:39](=[O:42])[NH:40][CH:41]=3)[C:27]3[CH:34]=[CH:33][C:32]([CH3:35])=[CH:31][C:28]=3[CH:29]=[CH:30][C:24]=2[CH:23]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C)C=O>[CH3:21][C:22]1[CH:45]=[CH:44][C:25]2[CH:26]([C:36]3[C:37](=[O:43])[NH:38][C:39](=[O:42])[N:40]([C:2]4[N:7]=[C:6]([NH:8][CH2:9][C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[C:5]([C:17]([O:19][CH3:20])=[O:18])=[CH:4][N:3]=4)[CH:41]=3)[C:27]3[CH:34]=[CH:33][C:32]([CH3:35])=[CH:31][C:28]=3[CH:29]=[CH:30][C:24]=2[CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 221172135-(2,8-Dimethyl-5h-dibenzo[a,d]cyclohepten-5-yl)-2,4(1h,3h)-pyrimidinedioneHCID 867556542-Chloro-4-[[[1,1-dimethylethoxy]carbonylmethyl]amino]-5-pyrimidinecarboxylic acid, methyl ester

生成物 1

HCID 867556552-[5-{2,8-Dimethyl-5H-dibenzo[a,d]cyclohepten-5-yl}-3,4-dihydro-2,4-dioxo-1(2H)-pyrimidinyl]-4-[[[1,1-dimethylethoxy]carbonylmethyl]amino]-5-pyrimidinecarboxylic acid, methyl ester

試薬・触媒・溶媒

1
HCID 6228Dimethylformamide溶媒

実験手順

A mixture of the product of step (ii) (0.52 g), the product of example 8 step (i) (0.5 g) and cesium carbonate (0.49 g) in dimethylformamide (15 ml) was heated at 70° C. After 3 hours, the reaction mixture was partitioned between 1M HCl and ethyl acetate. The organic phase was washed with water, dried (MgSO4) and evaporated under reduced pressure. Purification was by chromatography eluting with 3% methanol in chloroform. Yield 0.47 g.

後処理

  1. customthe reaction mixture was partitioned between 1M HCl and ethyl acetate
  2. washThe organic phase was washed with water
  3. dry with materialdried (MgSO4)
  4. customevaporated under reduced pressure
  5. customPurification
  6. washeluting with 3% methanol in chloroform

出典と根拠

ORDレコード
ord-32bbe3c4cd604d43ab12f69eb4092f6c
出典データセット
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06107297

反応ノート

読み込み中…

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