HCID 86615013, 화합물 → 5-(1-Hydroxyethyl)-N-methyl-N-propyl-isophthalamic acid ethyl ester

HRID 732565노트

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HRID 732565 반응식
[CH2:1]([O:3][C:4](=[O:20])[C:5]1[CH:17]=[C:16]([CH:18]=[O:19])[CH:15]=[C:7]([C:8]([N:10]([CH3:14])[CH2:11][CH2:12][CH3:13])=[O:9])[CH:6]=1)[CH3:2].[CH3:21][Mg]Br>C1COCC1>[CH2:1]([O:3][C:4](=[O:20])[C:5]1[CH:17]=[C:16]([CH:18]([OH:19])[CH3:21])[CH:15]=[C:7]([C:8]([N:10]([CH3:14])[CH2:11][CH2:12][CH3:13])=[O:9])[CH:6]=1)[CH3:2]

참가 물질

4

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HCID 86615013HCID 86615013, 화합물HCID 178418573HCID 178418573, 화합물

생성물 1

HCID 688153185-(1-Hydroxyethyl)-N-methyl-N-propyl-isophthalamic acid ethyl ester수율 59.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

Treat a solution of 5-formyl-N-methyl-N-propyl-isophthalamic acid ethyl ester (400 mg, 1.44 mmol) in THF (10 mL) at 0° C. with methylmagnesium bromide (3.0 M in diethyl ether, 0.58 mL, 1.73 mmol). Stir at 0° C. for 1 h and quench with saturated aqueous ammonium chloride solution. Extract with ethyl acetate (100 mL), dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 40:60 to 70:30 ethyl acetate:hexanes) to give the title compound (250 mg, 59%).

후처리

  1. customquench with saturated aqueous ammonium chloride solution
  2. extractionExtract with ethyl acetate (100 mL)
  3. dry with materialdry (magnesium sulfate)
  4. concentrationconcentrate
  5. custompurify
  6. wash(silica gel chromatography, eluting with 40:60 to 70:30 ethyl acetate:hexanes)

출처 및 근거

ORD 기록
ord-a35ab8fdb5864cc8bc7a88fbac9f2a5d
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585885B2

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