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Hydrochloric Acid → HCID 21034936, 화합물

HRID 1833134
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HRID 1833134 반응식
[CH2:1]([O:3][C:4](=[O:38])[N:5]([CH:12]([C:22]1[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[C:24]([O:30][CH2:31][C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH:23]=1)[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([O:20][CH3:21])[CH:15]=1)[CH2:6][CH:7](OC)OC)[CH3:2].Cl>CC(C)=O.O>[CH2:1]([O:3][C:4]([N:5]1[CH:6]=[CH:7][C:27]2[C:22](=[CH:23][C:24]([O:30][CH2:31][C:32]3[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=3)=[C:25]([O:28][CH3:29])[CH:26]=2)[CH:12]1[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([O:20][CH3:21])[CH:15]=1)=[O:38])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 21034940HCID 21034940, 화합물

생성물 1

HCID 21034936HCID 21034936, 화합물수율 48%

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

[1-(3-Benzyloxy-4-methoxy-phenyl)-2-(3-methoxy-phenyl)-ethyl]-(2,2-dimethoxy-ethyl)-carbamic acid ethyl ester (3.15 g, 6.01 mmol) was dissolved in acetone (125 mL) at 0° C., and 6M aqueous hydrochloric acid (25 mL) was added dropwise. After the addition was complete, the mixture was stored at 0° C. overnight (14 hours). The mixture was warmed to room temperature and stirred×4 hours. The mixture was cooled in an ice bath and diluted with water (150 mL). The mixture was extracted with ethyl acetate (3×60 mL). The combined organic extracts were washed with water (60 mL), saturated aqueous sodium chloride solution (60 mL) and dried over anhydrous magnesium sulfate. Concentration of the solvent gave an oily solid that was crystallized from ethyl acetate/hexanes to give 7-benzyloxy-6-methoxy-1-(3-methoxy-benzyl)-1H-isoquinoline-2-carboxylic acid ethyl ester (1.32 g, 2.87 mmol, 48%) as a white solid.

후처리

  1. additionAfter the addition
  2. custom(14 hours)
  3. temperatureThe mixture was cooled in an ice bath
  4. extractionThe mixture was extracted with ethyl acetate (3×60 mL)
  5. washThe combined organic extracts were washed with water (60 mL), saturated aqueous sodium chloride solution (60 mL)
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customConcentration of the solvent gave an oily solid
  8. customthat was crystallized from ethyl acetate/hexanes

출처 및 근거

ORD 기록
ord-855bef07717d48d892b03ff6cb42ccfd
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07067529B2

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