Cyclopropylamine → HCID 178418548、化合物

HRID 4570

反応式

HRID 4570 の反応式
[CH:1]([O-:6])([O-])[O:2][CH2:3][CH3:4].[F:7][C:8]1[CH:21]=[C:20]([N:22]2[CH:26]=[CH:25][CH:24]=[CH:23]2)[C:19]([F:27])=[CH:18][C:9]=1[C:10]([CH2:12][C:13](OCC)=O)=[O:11].[CH:28]1([NH2:31])[CH2:30][CH2:29]1>C(OC(=O)C)(=O)C>[CH:28]1([NH:31][CH:13]=[C:12]([C:10](=[O:11])[C:9]2[CH:18]=[C:19]([F:27])[C:20]([N:22]3[CH:23]=[CH:24][CH:25]=[CH:26]3)=[CH:21][C:8]=2[F:7])[C:1]([O:2][CH2:3][CH3:4])=[O:6])[CH2:30][CH2:29]1

参加物

5

反応物 3

HCID 69828CyclopropylamineHCID 53630039EthylorthoformateHCID 53691688Ethyl 2,5-difluoro-4-(pyrrol-1-yl)benzoylacetate

生成物 1

HCID 178418548HCID 178418548、化合物収率 36.1%

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

実験手順

1 g (0.0068 mol) of ethyl orthoformate is added to a solution of 1.1 g (0.00315 mol) of ethyl 2,5-difluoro-4-(pyrrol-1-yl)benzoylacetate in 3 ml of acetic anhydride and the mixture is refluxed for 3 hours. It is evaporated to dryness, the residue is dissolved in 10 ml of ethanol, 0.3 ml (0.0034 mol) of cyclopropylamine is added and the mixture is left at room temperature for 1 hour. It is evaporated to dryness and the oily residue is extracted with 3×30 ml of boiling hexane. The hexane fractions are concentrated to 20 ml and left for 12 hours at 5° C. to give 0.41 g of crystals melting at 90°-2° C.

後処理

  1. temperaturethe mixture is refluxed for 3 hours
  2. customIt is evaporated to dryness
  3. dissolutionthe residue is dissolved in 10 ml of ethanol
  4. customIt is evaporated to dryness
  5. extractionthe oily residue is extracted with 3×30 ml of boiling hexane
  6. concentrationThe hexane fractions are concentrated to 20 ml
  7. waitleft for 12 hours at 5° C.

出典と根拠

ORDレコード
ord-a4b80bde42b64cf99f5959c49c2e964f
出典データセット
uspto-grants-1988_02
特許番号
US04727080

関連ノート

読み込み中…