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Hydrochloric Acid → HCID 86746857, 화합물

HRID 248931
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HRID 248931 반응식
[CH2:1]([C:5]1[N:6]([CH2:16][C:17]2[CH:22]=[CH:21][C:20]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[C:29]#[N:30])=[CH:19][CH:18]=2)[CH:7]=[C:8]([CH2:10][CH2:11]C(OC)=O)[CH:9]=1)[CH2:2][CH2:3][CH3:4].[OH-:31].[Na+].Cl.[CH3:34][OH:35]>>[CH2:1]([C:5]1[N:6]([CH2:16][C:17]2[CH:18]=[CH:19][C:20]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[C:29]#[N:30])=[CH:21][CH:22]=2)[CH:7]=[C:8]([CH:10]([CH3:11])[C:34]([OH:35])=[O:31])[CH:9]=1)[CH2:2][CH2:3][CH3:4]
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참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 18946733HCID 18946733, 화합물

생성물 1

HCID 86746857HCID 86746857, 화합물

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온도
0 °C

실험 절차

To a solution of methyl 3-[2-(n-butyl)-1-(2"-cyanobiphenyl-4'-ylmethyl)pyrrol-4-yl]propionate (AG) (5.8 g) (prepared, e.g., as described in Preparation 23), in methanol (100 ml) was added 10% sodium hydroxide solution (35 ml), and the resulting solution was gently heated under reflux for 4 hours. After cooling to 0° C., the solution was acidified to pH 6 with hydrochloric acid solution (6N), and the product thoroughly extracted into methylene chloride. The combined methylene chloride extracts were washed with cold water, brine, and then dried with magnesium sulfate. Removal of the solvent under vacuum gave 3-[(2-(n-butyl)-1-(2"-cyanobiphenyl-4'-ylmethyl)pyrrol-4-yl]propionic acid (5.51 g), a compound of Formula (AH), as a slightly pinkish gum.

후처리

  1. temperaturethe resulting solution was gently heated
  2. temperatureunder reflux for 4 hours
  3. extractionthe product thoroughly extracted into methylene chloride
  4. washThe combined methylene chloride extracts were washed with cold water, brine
  5. dry with materialdried with magnesium sulfate
  6. customRemoval of the solvent under vacuum

출처 및 근거

ORD 기록
ord-90ed32b7618141b3b534f97a60e43dfe
출처 데이터셋
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05212195

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