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Water → 7-Chloro-5-((3-methyl-1H-indol-7-yl)amino)pyrido[3,4-d]pyridazin-4(3H)-one

HRID 629202
ノート
印刷プレビュー

反応式

HRID 629202 の反応式
Cl[C:2]1[C:7]2[C:8](=[O:12])[NH:9][N:10]=[CH:11][C:6]=2[CH:5]=[C:4]([Cl:13])[N:3]=1.CCN(C(C)C)C(C)C.[CH3:23][C:24]1[C:32]2[C:27](=[C:28]([NH2:33])[CH:29]=[CH:30][CH:31]=2)[NH:26][CH:25]=1.O>CS(C)=O>[Cl:13][C:4]1[N:3]=[C:2]([NH:33][C:28]2[CH:29]=[CH:30][CH:31]=[C:32]3[C:27]=2[NH:26][CH:25]=[C:24]3[CH3:23])[C:7]2[C:8](=[O:12])[NH:9][N:10]=[CH:11][C:6]=2[CH:5]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 186125633-methyl-1H-indol-7-amineHCID 887689205,7-Dichloropyrido[3,4-d]pyridazin-4(3H)-one

生成物 1

HCID 899724117-Chloro-5-((3-methyl-1H-indol-7-yl)amino)pyrido[3,4-d]pyridazin-4(3H)-one

試薬・触媒・溶媒 1

HCID 679
Dimethyl Sulfoxide
溶媒

反応条件

温度
140 °C

実験手順

To 5,7-dichloro-3H-pyrido[3,4-d]pyridazin-4-one (180 mg, 0.833 mmol) in DMSO (1 ml) in a sealable vial, was added DIPEA (0.189 ml, 1.083 mmol) and 3-methyl-1H-indol-7-amine (158 mg, 1.083 mmol). The vial was capped to close and the mixture heated on a sandbath at 140° C. for 1 h. The resultant mixture was poured into water (20 ml), and extracted with EtOAc (20 ml). Organic phase was washed with water then brine, dried over Na2SO4, then concentrated under vacuum. The residue was triterated with DCM, then collected by filtration and dried to give title compound as a yellow-mustard coloured solid.

後処理

  1. customThe vial was capped
  2. customto close
  3. extractionextracted with EtOAc (20 ml)
  4. washOrganic phase was washed with water
  5. dry with materialbrine, dried over Na2SO4
  6. concentrationconcentrated under vacuum
  7. filtrationcollected by filtration
  8. customdried

出典と根拠

ORDレコード
ord-0832cdb1abcb49aa8bc2962099f71763
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09315500B2

反応ノート

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