Triethylamine → HCID 54534260, 화합물

HRID 2073645노트

반응식

HRID 2073645 반응식
Br[C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=1.[C:11]([N:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1)(=[O:14])[CH:12]=[CH2:13].C(N(CC)CC)C>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.Cl>[C:6]([C:5]1[CH:9]=[CH:10][C:2]([CH:13]=[CH:12][C:11]([N:15]2[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]2)=[O:14])=[CH:3][CH:4]=1)([OH:8])=[O:7]

참가 물질

7

반응물 3

HCID 8471TriethylamineHCID 114644-Bromobenzoic acidHCID 3504731-(piperidin-1-yl)prop-2-en-1-one

생성물 1

HCID 54534260HCID 54534260, 화합물수율 98%

시약·촉매·용매 3

HCID 80271Tri-o-tolylphosphine촉매HCID 167845palladium(II) acetate촉매HCID 313Hydrochloric Acid용매

실험 절차

The acid chloride of the formula (500) and the corresponding free acid are novel and can be prepared as follows: 20.12 g (0.1 mol) of 4-bromobenzoic acid, 17.38 g (125 mmols) of acrylic acid piperidide, 25.28 g (250 mmols) of triethylamine, 0.224 g (1 mmol) of palladium acetate and 1.216 g (4 mmols) of tri-o-tolylphosphine are stirred at 115° C. for 15 minutes. The mixture is stirred with 300 ml of 2N hydrochloric acid and the crude product is filtered off. It is dissolved in 200 ml of 2N sodium hydroxide solution and the solution is filtered. 26 ml of 10N hydrochloric acid are added to the filtrate. The precipitate is filtered off, washed with water and dried. 25.27 g (98% of theory) of 4-carboxycinnamic acid piperidide are obtained in the form of white crystals; melting point 257.1° C.

후처리

  1. customcan be prepared
  2. filtrationthe crude product is filtered off
  3. dissolutionIt is dissolved in 200 ml of 2N sodium hydroxide solution
  4. filtrationthe solution is filtered
  5. addition26 ml of 10N hydrochloric acid are added to the filtrate
  6. filtrationThe precipitate is filtered off
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-1eb5309e52874a61a34d7a938de6d754
출처 데이터셋
uspto-grants-1990_04
특허 번호
US04918215

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