Hydrochloric Acid → 2-(1-Benzofuran-3-yl)acetic acid

HRID 1106896노트

반응식

HRID 1106896 반응식
C[O:2][C:3](=[O:14])[CH2:4][C:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[O:7][CH:6]=1.O.[OH-].[Li+].CO.Cl>O1CCCC1.O.C(OCC)C.CCCCCCC>[O:7]1[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[C:5]([CH2:4][C:3]([OH:14])=[O:2])=[CH:6]1

참가 물질

9

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 168937Lithium hydroxide, monohydrateHCID 10976279Methyl Benzofuran-3-acetate

생성물 1

HCID 27629402-(1-Benzofuran-3-yl)acetic acid

시약·촉매·용매 4

HCID 962Water용매2회HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매HCID 8900Heptane용매

실험 절차

A solution of Example 6 (6.23 g, 33 mmol) and lithium hydroxide monohydrate (1.45 g, 35 mmol) in tetrahydrofuran (50 mL), water (35 mL), and methanol (14 mL) was stirred for 6.5 hours at room temperature. Water (70 mL) was added, and the reaction mixture was acidified to pH 4 using 2 M HCl and extracted with dichloromethane (5×200 mL). The organics were dried (MgSO4) and the solvent removed in vacuo to give a brown solid. This was dissolved in diethyl ether, heptane was added, and the mixture was stirred overnight. Solvent was removed by syringe to give product as a pale brown solid, 27 mmol, 80%.

후처리

  1. extractionextracted with dichloromethane (5×200 mL)
  2. dry with materialThe organics were dried (MgSO4)
  3. customthe solvent removed in vacuo
  4. customto give a brown solid
  5. customSolvent was removed by syringe
  6. customto give product as a pale brown solid, 27 mmol, 80%

출처 및 근거

ORD 기록
ord-7b8b7bbf03ae41a4b7fbb33233ce36a3
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06057357

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