Triethylamine → HCID 15572887, 화합물

HRID 1154939노트

반응식

HRID 1154939 반응식
[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

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 62365Isobutyl chloroformateHCID 76688CyclohexanemethylamineHCID 12819271HCID 12819271, 화합물

생성물 1

HCID 15572887HCID 15572887, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-85c058f22a7949259d5a3c66e097e323
출처 데이터셋
uspto-grants-1981_11
특허 번호
US04298739

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