Hydrochloric Acid → HCID 22506876, 화합물

HRID 985601노트

반응식

HRID 985601 반응식
[I:1][CH2:2][C:3]1([CH3:21])[O:20][C:6]2=[C:7]([CH3:19])[C:8]3[CH2:9][C:10]([CH3:18])([CH3:17])[N:11](C=O)[C:12]=3[C:13]([CH3:14])=[C:5]2[CH2:4]1.Cl.C(=O)([O-])O.[Na+].O.C(OCC)(=O)C>CO>[I:1][CH2:2][C:3]1([CH3:21])[O:20][C:6]2=[C:7]([CH3:19])[C:8]3[CH2:9][C:10]([CH3:17])([CH3:18])[NH:11][C:12]=3[C:13]([CH3:14])=[C:5]2[CH2:4]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 22506878HCID 22506878, 화합물HCID 22728543Water ethylacetate

생성물 1

HCID 22506876HCID 22506876, 화합물수율 98%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 2,3,6,7-tetrahydro-2-(iodomethyl)-2,4,6,6,8-pentamethyl-5H-furo[2,3-f]indole-5-carbaldehyde (2.42 g, 6.06 mmol) in methanol (10 ml) was added concentrated hydrochloric acid (3 ml), and heated under reflux for 2.5 hours under nitrogen atmosphere. The reaction mixture was added dropwise to a mixture of sodium hydrogen carbonate (3.7 g, 44 mmol) with water-ethyl acetate, neutralized and extracted three times with ethyl acetate. The organic layers were combined, washed with water and saturated brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure to obtain 2.20 g of the title compound.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 2.5 hours under nitrogen atmosphere
  3. extractionextracted three times with ethyl acetate
  4. washwashed with water and saturated brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-aef4d9e3002e42e894949aeeef8b6547
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06872718B1

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