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Water → N-allyl-2-chloro-8-(4-fluorophenyl)-N,6-dimethyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine

HRID 474277
ノート
印刷プレビュー

反応式

HRID 474277 の反応式
[Cl:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[CH2:11][N:10]([CH3:12])[CH2:9][CH:8]([C:13]3[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=3)[C:6]=2[N:7]=1.[CH3:21][NH:22][CH2:23][CH:24]=[CH2:25].O>CN1C(=O)CCC1>[CH2:23]([N:22]([CH3:21])[C:4]1[C:5]2[CH2:11][N:10]([CH3:12])[CH2:9][CH:8]([C:13]3[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=3)[C:6]=2[N:7]=[C:2]([Cl:1])[N:3]=1)[CH:24]=[CH2:25]
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 962WaterHCID 69391N-MethylallylamineHCID 580753632,4-Dichloro-8-(4-fluorophenyl)-6-methyl-5,6,7,8-tetrahydropyrido[4,3-D]pyrimidine

生成物 1

HCID 86668120N-allyl-2-chloro-8-(4-fluorophenyl)-N,6-dimethyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine収率 100%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

The mixture of 2,4-dichloro-8-(4-fluorophenyl)-6-methyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (Preparation V, 408 mg, 1.307 mmol) in NMP (13 mL) was added N-methylprop-2-en-1-amine (465 mg, 6.53 mmol). The resulting reaction mixture was stirred at rt overnight. Water (50 mL) was added to the mixture and stirred for 30 min. The mixture was filtered to get a light tan solid which was dried and purified by flash column chromatography eluting with 30 to 100% EtOAc/Hexane to get N-allyl-2-chloro-8-(4-fluorophenyl)-N,6-dimethyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine (453 mg, 100% yield). LC-MS (M+H)+=347.1.

後処理

  1. customThe resulting reaction mixture
  2. stirringstirred for 30 min
  3. filtrationThe mixture was filtered
  4. customto get a light tan solid which
  5. customwas dried
  6. custompurified by flash column chromatography
  7. washeluting with 30 to 100% EtOAc/Hexane

出典と根拠

ORDレコード
ord-2c4a11379c1b49f49a229c1e0a892e6d
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08637523B2

反応ノート

読み込み中…

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