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Hydrochloric Acid → HCID 69676423, 화합물

HRID 919617
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HRID 919617 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][CH2:10][C:11]([N:13]2[CH2:18][CH2:17][CH:16]([CH3:19])[CH:15]([NH:20]C(=O)OC(C)(C)C)[CH2:14]2)=[O:12])[CH:5]=[C:6]([Cl:8])[CH:7]=1.Cl>O1CCOCC1>[NH2:20][CH:15]1[CH:16]([CH3:19])[CH2:17][CH2:18][N:13]([C:11](=[O:12])[CH2:10][NH:9][C:4]2[CH:5]=[C:6]([Cl:8])[CH:7]=[C:2]([Cl:1])[CH:3]=2)[CH2:14]1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 69676422HCID 69676422, 화합물

생성물 1

HCID 69676423HCID 69676423, 화합물수율 87.8%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

Tert-butyl 1-(2-(3,5-dichlorophenylamino)acetyl)-4-methylpiperidin-3-ylcarbamate (150 mg, 0.36 mmol) was treated with dioxane.HCl (5 mL) at rt for 2 h. The solvent was concentrated in vacuo, the resulting residue was dissolved in water (10 mL) and treated with solid NaHCO3. The aqueous solution was extracted with EtOAc (3×25 mL) and the combined organic layers were dried over Na2SO4, concentrated in vacuo to yield the titled intermediate (100 mg, 87%), which was used next without further purification. LC-MS: m/z [M+1]=316.

후처리

  1. concentrationThe solvent was concentrated in vacuo
  2. dissolutionthe resulting residue was dissolved in water (10 mL)
  3. additiontreated with solid NaHCO3
  4. extractionThe aqueous solution was extracted with EtOAc (3×25 mL)
  5. dry with materialthe combined organic layers were dried over Na2SO4
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-ecb6afb903c24e41b85b3d38b6367036
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09273028B2

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