Water → 4-(2-Isopropoxy-3-methyl-benzoylamino)-tetrahydro-thiopyran-4-carboxylic acid

HRID 1047686노트

반응식

HRID 1047686 반응식
C[O:2][C:3]([C:5]1([NH:11][C:12](=[O:24])[C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([CH3:19])[C:14]=2[O:20][CH:21]([CH3:23])[CH3:22])[CH2:10][CH2:9][S:8][CH2:7][CH2:6]1)=[O:4].[OH-].[K+].O>CCO>[CH:21]([O:20][C:14]1[C:15]([CH3:19])=[CH:16][CH:17]=[CH:18][C:13]=1[C:12]([NH:11][C:5]1([C:3]([OH:4])=[O:2])[CH2:6][CH2:7][S:8][CH2:9][CH2:10]1)=[O:24])([CH3:23])[CH3:22]

참가 물질

5

반응물 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 593141894-(2-Isopropoxy-3-methyl-benzoylamino)-tetrahydro-thiopyran-4-carboxylic acid methyl ester

생성물 1

HCID 593141484-(2-Isopropoxy-3-methyl-benzoylamino)-tetrahydro-thiopyran-4-carboxylic acid수율 96%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The mixture of 4-(2-isopropoxy-3-methyl-benzoylamino)-tetrahydro-thiopyran-4-carboxylic acid methyl ester (28) (75 mg, 0.21 mmol) and KOH (500 mg, 8.9 mmol) is dissolved in EtOH (5 mL) and water (0.5 mL) under a water bath. The water bath is removed when KOH is completely dissolved and the resulting reaction solution is stirred at RT for 8 h. After concentration in vacuo, the residue is dissolved in water (20 mL) and acidified with conc. HCl until no more precipitate came out of the water. The precipitate is filtered to give a pure product (29) as a pale yellow solid (68 mg, 94%).

후처리

  1. customThe water bath is removed when KOH
  2. dissolutionis completely dissolved
  3. customthe resulting reaction solution
  4. concentrationAfter concentration in vacuo
  5. dissolutionthe residue is dissolved in water (20 mL)
  6. filtrationThe precipitate is filtered

출처 및 근거

ORD 기록
ord-4405809c70764717a31f95d8098d0567
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08569535B2

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