2-Benzoylbenzoic Acid → HCID 21398396、化合物

HRID 1439173ノート

反応式

HRID 1439173 の反応式
[C:1]([C:9]1[CH:17]=[CH:16][CH:15]=[CH:14][C:10]=1[C:11]([OH:13])=O)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:18]([NH:21][CH2:22][CH2:23][CH2:24][NH2:25])[CH2:19][CH3:20].ClC1C=CC=CC=1Cl>O>[CH2:18]([N:21]1[C:1]2([C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[C:9]3[C:10]([C:11](=[O:13])[N:25]2[CH2:24][CH2:23][CH2:22]1)=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH2:19][CH3:20]

参加物

5

反応物 3

HCID 68132-Benzoylbenzoic AcidHCID 72391,2-DichlorobenzeneHCID 90250N-Propylpropane-1,3-diamine

生成物 1

HCID 21398396HCID 21398396、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

22.6 Parts of o-benzoyl-benzoic acid and 11.6 parts of N-propyl-1,3-propanediamine are haeted within 11/2 hours with 50 parts by volume of o-dichlorobenzene until the boiling point of the latter is attained. Almost the theoretical amount of reaction water is azeotropically distilled off. The clear solution is evaporated to dryness in vacuo, the oily residue is dissolved in ethyl acetate and crystallised by the dropwise addition of pentane. In this way, 1-propyl-10b-phenyl-1,3,4,10b-tetrahydro-pyrimido[2,1-a]isoindol-6(2H)-one is obtained of the formula ##STR19## M.P. 135°-137°. 1-Ethyl-10b-phenyl-1,3,4,10b-tetrahydro-pyrimido[2,1-a]isoindol -6(2H)-one is obtained in the same manner from o-benzoyl-benzoic acid and N-ethyl-1,3-propanediamine. M.P. 131°-133°.

後処理

  1. custom2 hours
  2. distillationis azeotropically distilled off
  3. customThe clear solution is evaporated to dryness in vacuo
  4. dissolutionthe oily residue is dissolved in ethyl acetate
  5. customcrystallised by the dropwise addition of pentane

出典と根拠

ORDレコード
ord-9ec9e32eb84549c7a900d2c8f12a4ce5
出典データセット
uspto-grants-1977_11
特許番号
US04058529

反応ノート

読み込み中…