Lithium Hydroxide → HCID 86669558, 화합물

HRID 524433노트

반응식

HRID 524433 반응식
[CH:1]1([S:4]([C:7]2[CH:12]=[CH:11][C:10]([CH:13]([O:34][C@@H:35]3[CH2:39][CH2:38][O:37][CH2:36]3)[C:14]([NH:16][C:17]3[S:18][C:19]([O:22][C:23]4[CH:24]=[CH:25][C:26]([CH3:33])=[C:27]([CH:32]=4)[C:28]([O:30]C)=[O:29])=[CH:20][N:21]=3)=[O:15])=[CH:9][CH:8]=2)(=[O:6])=[O:5])[CH2:3][CH2:2]1.[Li+].[OH-]>C1COCC1.CO>[CH:1]1([S:4]([C:7]2[CH:12]=[CH:11][C:10]([CH:13]([O:34][C@@H:35]3[CH2:39][CH2:38][O:37][CH2:36]3)[C:14]([NH:16][C:17]3[S:18][C:19]([O:22][C:23]4[CH:24]=[CH:25][C:26]([CH3:33])=[C:27]([CH:32]=4)[C:28]([OH:30])=[O:29])=[CH:20][N:21]=3)=[O:15])=[CH:9][CH:8]=2)(=[O:6])=[O:5])[CH2:2][CH2:3]1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 86669552HCID 86669552, 화합물

생성물 1

HCID 86669558HCID 86669558, 화합물수율 88.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

5-[2-[[2-(4-cyclopropylsulfonylphenyl)-2-[(3R)-tetrahydrofuran-3-yl]oxy-acetyl]amino]thiazol-5-yl]oxy-2-methyl-benzoic acid methyl ester (Example A3; 0.300 g, 0.524 mmol) was taken in THF(4 mL) and MeOH (0.1 mL), to it was added aqueous solution of LiOH (0.110 g, 2.62 mmol in 7 mL water) and stirred for 1-4 h at room temperature. After completion of the reaction, organic solvent was removed under reduced pressure. The aqueous layer was washed with diisopropyl ether then acidified with 1 N HCl to pH 2. The solid formed was filtered, washed with water, followed by washing with diisopropyl ether & dried under vacuum to get the title compound (0.260 g).

후처리

  1. customAfter completion of the reaction, organic solvent
  2. customwas removed under reduced pressure
  3. washThe aqueous layer was washed with diisopropyl ether
  4. customThe solid formed
  5. filtrationwas filtered
  6. washwashed with water
  7. washby washing with diisopropyl ether
  8. customdried under vacuum

출처 및 근거

ORD 기록
ord-c6d7a78d83bb46ebbc685ce330c95415
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09340506B2

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