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Salmeterol → Salmeterol 4-phenylcinnamate

HRID 2220126
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HRID 2220126 반응식
[C:1]1([C:7]2[CH:17]=[CH:16][C:10]([CH:11]=[CH:12][C:13]([OH:15])=[O:14])=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:18]1[CH:19]=[CH:20][C:21]([CH2:24][CH2:25][CH2:26][CH2:27][O:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][NH:35][CH2:36][CH:37]([OH:47])[C:38]2[CH:39]=[CH:40][C:41]([OH:46])=[C:42]([CH2:44][OH:45])[CH:43]=2)=[CH:22][CH:23]=1>C(OCC)(=O)C>[CH:18]1[CH:19]=[CH:20][C:21]([CH2:24][CH2:25][CH2:26][CH2:27][O:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][NH:35][CH2:36][CH:37]([OH:47])[C:38]2[CH:39]=[CH:40][C:41]([OH:46])=[C:42]([CH2:44][OH:45])[CH:43]=2)=[CH:22][CH:23]=1.[C:1]1([C:7]2[CH:8]=[CH:9][C:10]([CH:11]=[CH:12][C:13]([O-:15])=[O:14])=[CH:16][CH:17]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 5152SalmeterolHCID 254923-(4-Phenylphenyl)prop-2-enoic acid

생성물 1

HCID 86760723Salmeterol 4-phenylcinnamate수율 1,226.2%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

1.35 g (6 mmol) of 4-phenylcinnamic acid is dissolved by refluxing in 75 mL of ethyl acetate. To this solution is added a warm solution of 2.5 g (6 mmol) of salmeterol in 25 mL of ethyl acetate. The solution is allowed to cool and stirred for 16 hours at room temperature. The suspension is filtered, the precipitate is washed with ethyl acetate and tert-butylmethylether and dried in vacuo at 25° C.-30° C. 47 g of the title compound are obtained as a colorless solid. Melting point: 109° C. 2.2. Salmeterol-5-(2,4-difluorophenyl)salicylate Salt 2c

후처리

  1. temperatureto cool
  2. filtrationThe suspension is filtered
  3. washthe precipitate is washed with ethyl acetate and tert-butylmethylether
  4. customdried in vacuo at 25° C.-30° C

출처 및 근거

ORD 기록
ord-1592578a693f4b61a603ac9d25977977
출처 데이터셋
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07417051B2

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