3-Amino-1-propanol → HCID 53693826, 화합물

HRID 234219노트

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HRID 234219 반응식
CO[C:3]([C@H:5]1[NH:18][C:17](=[S:19])[CH2:16][CH2:15][CH2:14][CH2:13][O:12][C:11](=[O:20])[C:10]2[C:21]([CH3:28])=[C:22]([O:26][CH3:27])[CH:23]=[C:24]([OH:25])[C:9]=2[CH2:8][S:7][CH2:6]1)=[O:4].[NH2:29][CH2:30][CH2:31][CH2:32][OH:33]>CO.C(OCC)(=O)C>[OH:33][CH2:32][CH2:31][CH2:30][NH:29][C:3]([C@H:5]1[NH:18][C:17](=[S:19])[CH2:16][CH2:15][CH2:14][CH2:13][O:12][C:11](=[O:20])[C:10]2[C:21]([CH3:28])=[C:22]([O:26][CH3:27])[CH:23]=[C:24]([OH:25])[C:9]=2[CH2:8][S:7][CH2:6]1)=[O:4]

참가 물질

5

반응물 2

HCID 90863-Amino-1-propanolHCID 9823853Methyl (4R)-1,3,4,5,6,7,8,9,10,12-decahydro-16-hydroxy-14-methoxy-13-methyl-12-oxo-6-thioxo-11,2,5-benzoxathiaazacyclotetradecine-4-carboxylate

생성물 1

HCID 53693826HCID 53693826, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

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온도
50 °C

실험 절차

A solution of 43 mg of the product of Example 23 in a mixture of 0.5 ml of methanol and 0.5 ml of 3-amino-propanol was heated to 50° C. 20 min. The mixture was diluted with ethyl acetate and washed with 1N hydrochloric acid and water. The organic layer was dried over sodium sulfate and evaporated in vacuo and the solid residue was recrystallized from ethyl acetate/hexane to afford 12 mg (R)-16-hydroxy-14-methoxy-13-methyl-12-oxo-6-thioxo-1,3,4,5,6,7,8,9,10,12-decahydro-11,2,5-benzoxathiaazacyclotetradecine-4-carboxylic acid 3-hydroxy-propylamide as a white solid.

후처리

  1. custom20 min
  2. washwashed with 1N hydrochloric acid and water
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. customevaporated in vacuo
  5. customthe solid residue was recrystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-a8aaefab581a4b5ba6eee3801613b6fe
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05594135

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