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Hydrochloric Acid → (S)-2-amino-2-(3-fluoro-5-iodophenyl)ethanol hydrochloride

HRID 596038
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HRID 596038 반응식
[F:1][C:2]1[CH:3]=[C:4]([C@H:9]([NH:12]C(=O)OC(C)(C)C)[CH2:10][OH:11])[CH:5]=[C:6]([I:8])[CH:7]=1.[ClH:20].O1CCOCC1>C(Cl)Cl>[ClH:20].[NH2:12][C@@H:9]([C:4]1[CH:5]=[C:6]([I:8])[CH:7]=[C:2]([F:1])[CH:3]=1)[CH2:10][OH:11]
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 118054565(S)-tert-butyl (1-(3-fluoro-5-iodophenyl)-2-hydroxyethyl)carbamate

생성물 1

HCID 118045249(S)-2-amino-2-(3-fluoro-5-iodophenyl)ethanol hydrochloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

(S)-tert-butyl (1-(3-fluoro-5-iodophenyl)-2-hydroxyethyl)carbamate (2.507 g, 6.58 mmol) was dissolved in DCM (60 mL) and treated with 4 N HCl in dioxane (4.93 mL, 19.73 mmol). The mixture was stirred overnight at room temperature. After the majority of the solvent was evaporated carefully in vacuo, the slurry was triturated with Et2O to afford 1.525 g of a fine white HCl salt of (S)-2-amino-2-(3-fluoro-5-iodophenyl)ethanol (72%), which was isolated by suction filtration. LCMS (m/z): 282.4 (MH+), 0.46 min.

후처리

  1. customAfter the majority of the solvent was evaporated carefully in vacuo
  2. customthe slurry was triturated with Et2O

출처 및 근거

ORD 기록
ord-364c6127db4b40d18a17a111bef4af86
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09242996B2

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