Triethylamine → {{8-[5-(4-Fluorophenyl)-2-pentyl]-10-hydroxy-5,5-dimethyl-1,2,3,4-tetrahydro-5H-[1]benzopyrano[4,3-c]pyridin-2-yl}acetyl}urea

HRID 427093노트

반응식

HRID 427093 반응식
Cl[CH2:2][C:3]([NH:5][C:6]([NH2:8])=[O:7])=[O:4].[F:9][C:10]1[CH:15]=[CH:14][C:13]([CH2:16][CH2:17][CH2:18][CH:19]([C:21]2[CH:26]=[C:25]([OH:27])[C:24]3[C:28]4[CH2:29][NH:30][CH2:31][CH2:32][C:33]=4[C:34]([CH3:37])([CH3:36])[O:35][C:23]=3[CH:22]=2)[CH3:20])=[CH:12][CH:11]=1.C(N(CC)CC)C>CN(C)C=O>[F:9][C:10]1[CH:15]=[CH:14][C:13]([CH2:16][CH2:17][CH2:18][CH:19]([C:21]2[CH:26]=[C:25]([OH:27])[C:24]3[C:28]4[CH2:29][N:30]([CH2:2][C:3]([NH:5][C:6]([NH2:8])=[O:7])=[O:4])[CH2:31][CH2:32][C:33]=4[C:34]([CH3:36])([CH3:37])[O:35][C:23]=3[CH:22]=2)[CH3:20])=[CH:12][CH:11]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 78516(2-Chloroacetyl)ureaHCID 128007415,5-dimethyl-8-[5-(4-fluorophenyl)-2-pentyl]-10-hydroxy-1,2,3,4-tetrahydro-5H-[1]benzopyrano[3,4-d]pyridine

생성물 1

HCID 44327286{{8-[5-(4-Fluorophenyl)-2-pentyl]-10-hydroxy-5,5-dimethyl-1,2,3,4-tetrahydro-5H-[1]benzopyrano[4,3-c]pyridin-2-yl}acetyl}urea

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

A solution of 1.50 g. (0.011 mole) of chloroacetyl urea in 20 ml. of dimethylformamide was added dropwise to a stirred solution of 3.95 g. (0.01 mole) of 8-[5-(4-fluorophenyl)-2-pentyl]-10-hydroxy-5,5-dimethyl-1,2,3,4-tetrahydro-5H-[1]benzopyrano[4,3-c]pyridine in 25 ml. of dimethylformamide and 1.11 g. (0.011 mole) of triethylamine. After stirring at room temperature for 22 hours, the mixture was diluted with 45 ml. of water and extracted with ether. The combined ether extracts were washed with water, dried over anhydrous sodium sulfate, and evaporated in vacuo. The residue was recrystallized from acetonitrile, m.p. 133°-134°.

후처리

  1. additionthe mixture was diluted with 45 ml
  2. extractionof water and extracted with ether
  3. washThe combined ether extracts were washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customevaporated in vacuo
  6. customThe residue was recrystallized from acetonitrile, m.p. 133°-134°

출처 및 근거

ORD 기록
ord-0f8f54fdfea04215a741ec2ea6cace57
출처 데이터셋
uspto-grants-1979_10
특허 번호
US04172943

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