4-Hydroxypyrrolidine → 11-Ethyl-2-(3-hydroxypyrrolidin-1-yl)-4-methyl-5,11-dihydro-6H-dipyrido[2,3-e:3',2'-b][1,4]diazepin-6-one

HRID 53543

反応式

HRID 53543 の反応式
Cl[C:2]1[CH:3]=[C:4]([CH3:20])[C:5]2[NH:6][C:7](=[O:19])[C:8]3[CH:18]=[CH:17][CH:16]=[N:15][C:9]=3[N:10]([CH2:13][CH3:14])[C:11]=2[N:12]=1.[OH:21][CH:22]1[CH2:26][CH2:25][NH:24][CH2:23]1>O>[CH2:13]([N:10]1[C:9]2[N:15]=[CH:16][CH:17]=[CH:18][C:8]=2[C:7](=[O:19])[NH:6][C:5]2[C:4]([CH3:20])=[CH:3][C:2]([N:24]3[CH2:25][CH2:26][CH:22]([OH:21])[CH2:23]3)=[N:12][C:11]1=2)[CH3:14]

参加物

4

反応物 2

HCID 982104-HydroxypyrrolidineHCID 463144Dipyridodiazepinone deriv. 15

生成物 1

HCID 46354911-Ethyl-2-(3-hydroxypyrrolidin-1-yl)-4-methyl-5,11-dihydro-6H-dipyrido[2,3-e:3',2'-b][1,4]diazepin-6-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
170 °C

実験手順

A suspension of the 2-chloro-5,11-dihydro-11-ethyl-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.14 g) in 3-hydroxypyrrolidine (0.29 g) in an open test tube was heated at 170° C. for 30 minutes. After cooling to room temperature the mixture was diluted with water and extracted with ethyl acetate. The organic phase was washed, dried, and evaporated. Chromatography over silica gel with ethyl acetate gave the title compound, which crystallized from ethyl acetate. Yield, 0.12 g, m.p. 131°-134° C.

後処理

  1. temperatureAfter cooling to room temperature the mixture
  2. extractionextracted with ethyl acetate
  3. washThe organic phase was washed
  4. customdried
  5. customevaporated

出典と根拠

ORDレコード
ord-85aae3c011414557809e137dd866b50d
出典データセット
uspto-grants-1997_04
特許番号
US05620974

関連ノート

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