Tetrahydrofuran → HCID 23509023, 화합물

HRID 1884253

반응식

HRID 1884253 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:17][CH2:18][NH2:19])[CH:6]=[CH:7][C:8]=1[O:9][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(N(CC)CC)C.O1CCCC1.[CH:32]1[C:41]2[CH2:40][CH2:39][CH2:38][CH2:37][C:36]=2[CH:35]=[CH:34][C:33]=1[CH2:42][C:43](Cl)=[O:44]>O>[CH2:10]([O:9][C:8]1[CH:7]=[CH:6][C:5]([CH2:17][CH2:18][NH:19][C:43](=[O:44])[CH2:42][C:33]2[CH:34]=[CH:35][C:36]3[CH2:37][CH2:38][CH2:39][CH2:40][C:41]=3[CH:32]=2)=[CH:4][C:3]=1[O:2][CH3:1])[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 200382Phenethylamine, 4-(benzyloxy)-3-methoxy-HCID 23508965(5,6,7,8-Tetrahydronaphthalen-2-yl)acetyl chloride

생성물 1

HCID 23509023HCID 23509023, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

8.01 g (31.2 mmol) of crude 2-(3-methoxy-4-benzyloxyphenyl)ethylamine, 3.78 g (37.4 mmol) of triethylamine and 80 ml of tetrahydrofuran were mixed and cooled to 0° C. and then (5,6,7,8-tetrahydronaphthalen-2-yl)acetyl chloride was added dropwise thereto. The mixture was stirred at 0° C. for 30 minutes and further at room temperature for 2 hours. Water was added to the reaction mixture, which was followed by extracted with ethyl acetate, washed with 5% hydrochloric acid and then saturated brine, dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was subjected to silica gel column chromatography (eluent, hexane:ethyl acetate=1:1) to give 8.3 g of N-[2-(4-benzyloxy-3-methoxyphenyl)ethyl]-2-(5,6,7,8-tetrahydronaphthalen-2-yl)acetamide.

후처리

  1. extractionby extracted with ethyl acetate
  2. washwashed with 5% hydrochloric acid
  3. dry with materialsaturated brine, dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-b9be2b3a757c49ffa25f02056c42ac50
출처 데이터셋
uspto-grants-2004_07
특허 번호
US06762321B2

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