Triethylamine → HCID 15572887、化合物

HRID 1154939ノート

反応式

HRID 1154939 の反応式
[C:1]([CH2:4][CH2:5][CH2:6][O:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[NH:14][C:13](=[O:18])[CH2:12][CH2:11]2)([OH:3])=O.C(N(CC)CC)C.ClC(OCC(C)C)=O.[CH:34]1([CH2:40][NH2:41])[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]1>O.CN(C)C=O>[CH:34]1([CH2:40][NH:41][C:1]([CH2:4][CH2:5][CH2:6][O:7][C:8]2[CH:9]=[C:10]3[C:15](=[CH:16][CH:17]=2)[NH:14][C:13](=[O:18])[CH2:12][CH2:11]3)=[O:3])[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]1

参加物

7

反応物 4

HCID 8471TriethylamineHCID 62365Isobutyl chloroformateHCID 76688CyclohexanemethylamineHCID 12819271HCID 12819271、化合物

生成物 1

HCID 15572887HCID 15572887、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

2.5 Grams of 6-(3-carboxy)propoxy-3,4-dihydrocarbostyril and 1.6 ml of triethylamine are added to 150 ml of dimethylformamide, and the mixture is further added dropwise with 1.3 ml of isobutyl chloroformate under external ice cooling and agitation while maintaining the internal temperature at 10° to 20° C. After this dropwise addition, the mixture is agitated at room temperature for 30 minutes, added with 1.3 ml of cyclohexylmethylamine and further agitated for 1 hour. After the reaction, the reaction solution is poured into about 1 liter of water and the precipitated crystals are filtered out and washed with water. The obtained crystals are dried and recrystallized from chloroform-petroleum ether to obtain 3.0 g of 6-{3-[N-(cyclohexylmethyl)aminocarbonyl]propoxy}-3,4-dihydrocarbostyril in the form of colorless needle-like crystals with m.p. of 170°-172° C.

後処理

  1. temperatureagitation while maintaining the internal temperature at 10° to 20° C
  2. additionAfter this dropwise addition
  3. stirringfurther agitated for 1 hour
  4. customAfter the reaction
  5. filtrationthe precipitated crystals are filtered out
  6. washwashed with water
  7. customThe obtained crystals are dried
  8. customrecrystallized from chloroform-petroleum ether

出典と根拠

ORDレコード
ord-85c058f22a7949259d5a3c66e097e323
出典データセット
uspto-grants-1981_11
特許番号
US04298739

反応ノート

読み込み中…