N,N-Diethyl-1,4-butanediamine → 1-Cyclopropyl-7-(4-diethylamino-butylamino)-3-(2,6-difluoro-3,5-dimethoxy-phenyl)-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one

HRID 459972

反応式

HRID 459972 の反応式
[CH:1]1([N:4]2[C:9]3=[N:10][C:11](S(C)=O)=[N:12][CH:13]=[C:8]3[CH2:7][N:6]([C:17]3[C:22]([F:23])=[C:21]([O:24][CH3:25])[CH:20]=[C:19]([O:26][CH3:27])[C:18]=3[F:28])[C:5]2=[O:29])[CH2:3][CH2:2]1.[CH2:30]([N:32]([CH2:38][CH3:39])[CH2:33][CH2:34][CH2:35][CH2:36][NH2:37])[CH3:31].C(OCC)(=O)C.C(O)C.C(N(CC)CC)C>O1CCOCC1>[CH:1]1([N:4]2[C:9]3=[N:10][C:11]([NH:37][CH2:36][CH2:35][CH2:34][CH2:33][N:32]([CH2:38][CH3:39])[CH2:30][CH3:31])=[N:12][CH:13]=[C:8]3[CH2:7][N:6]([C:17]3[C:22]([F:23])=[C:21]([O:24][CH3:25])[CH:20]=[C:19]([O:26][CH3:27])[C:18]=3[F:28])[C:5]2=[O:29])[CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 117976N,N-Diethyl-1,4-butanediamineHCID 184446941-cyclopropyl-3-(2,6-difluoro-3,5-dimethoxy-phenyl)-7-methanesulfinyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-oneHCID 22328969EtOH ethyl acetate triethylamine

生成物 1

HCID 103238501-Cyclopropyl-7-(4-diethylamino-butylamino)-3-(2,6-difluoro-3,5-dimethoxy-phenyl)-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one収率 83%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Using Procedure K, 0.63 g (1.48 mmol) of 1-cyclopropyl-3-(2,6-difluoro-3,5-dimethoxy-phenyl)-7-methanesulfinyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one and 4-(diethylamino)butylamine in 20 mL of dioxane were reacted. Chromatography with 9:1:0.5 ethyl acetate/ethanol/triethylamine gave 0.62 g (83%) of the title compound as a solid: mp 139° C.–141° C. MS (APCI) (m+1)/z 505.2. Analysis calculated for C25H34N6F2O3: C, 59.51; H, 6.79; N, 16.66. Found: C, 59.56; H, 6.77; N, 16.49.

後処理

  1. customwere reacted

出典と根拠

ORDレコード
ord-ad02a537a6d64c6a8d1abf44a0cc9f76
出典データセット
uspto-grants-2007_03
特許番号
US07196090B2

関連ノート

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