Hydrochloric Acid → HCID 9840634, 화합물

HRID 1354814노트

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HRID 1354814 반응식
[OH-].[Na+].C([O:10][C:11](=[O:34])[C:12]1[CH:17]=[CH:16][C:15]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[CH:14][C:13]=1[O:26][CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)C1C=CC=CC=1.Cl>CO>[CH2:27]([O:26][C:13]1[CH:14]=[C:15]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:16]=[CH:17][C:12]=1[C:11]([OH:34])=[O:10])[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 15087000Phenylmethyl 2,4-bis(phenylmethoxy)benzoate

생성물 1

HCID 9840634HCID 9840634, 화합물수율 38.92%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
65 °C

실험 절차

NaOH (1 N) (150 mL) was added to compound 36 (4.3 g) in MeOH (50 mL). The reaction mixture was heated to 65° C. with stirring for 48 h. After the reaction mixture was cooled down to room temperature, 1.0 M HCl (200 mL) was added to neutralize the reaction mixture. The solvent was concentrated under reduced pressure. The residue was extracted with CHCl3 and H2O. The combined organic layer was dried over MgSO4. After the MgSO4 was filtered off, the solvent was removed under reduced pressure. The residue was purified by flash chromatography to give the compound 37 (1.3 g) as a solid with total yield of 38.92% for 2 steps. LC-MS (ESI): m/e=335.2 [M+1]+

후처리

  1. temperatureAfter the reaction mixture was cooled down to room temperature
  2. concentrationThe solvent was concentrated under reduced pressure
  3. extractionThe residue was extracted with CHCl3 and H2O
  4. dry with materialThe combined organic layer was dried over MgSO4
  5. filtrationAfter the MgSO4 was filtered off
  6. customthe solvent was removed under reduced pressure
  7. customThe residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-385dc4a5f9c64d6d9acfe15963fdfeec
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07223759B2

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