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Thionyl Chloride → methyl 3-(3-(3-(chloromethyl)pyridin-2-yl)-1H-pyrazol-1-yl)propanoate hydrochloride

HRID 1471758
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반응식

HRID 1471758 반응식
O[CH2:2][C:3]1[C:4]([C:9]2[CH:13]=[CH:12][N:11]([CH2:14][CH2:15][C:16]([O:18][CH3:19])=[O:17])[N:10]=2)=[N:5][CH:6]=[CH:7][CH:8]=1.O=S(Cl)[Cl:22]>C(Cl)Cl>[ClH:22].[Cl:22][CH2:2][C:3]1[C:4]([C:9]2[CH:13]=[CH:12][N:11]([CH2:14][CH2:15][C:16]([O:18][CH3:19])=[O:17])[N:10]=2)=[N:5][CH:6]=[CH:7][CH:8]=1
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참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 86690795methyl 3-(3-(3-(hydroxymethyl)pyridin-2-yl)-1H-pyrazol-1-yl)propanoate

생성물 1

HCID 86690796methyl 3-(3-(3-(chloromethyl)pyridin-2-yl)-1H-pyrazol-1-yl)propanoate hydrochloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To methyl 3-(3-(3-(hydroxymethyl)pyridin-2-yl)-1H-pyrazol-1-yl)propanoate (51 mg, 0.20 mmol) in DCM (5 mL) was added SOCl2 (1.0 mL) at rt. The reaction mixture was stirred at rt for 4 h and concentrated to dryness. The crude solid was suspended in toluene and concentrated to dryness. The process was repeated three times and dried under vacuum to give methyl 3-(3-(3-(chloromethyl)pyridin-2-yl)-1H-pyrazol-1-yl)propanoate hydrochloride (63 mg) as an off-white solid, which was used for next step without further purification.

후처리

  1. concentrationconcentrated to dryness
  2. concentrationconcentrated to dryness
  3. customdried under vacuum

출처 및 근거

ORD 기록
ord-5993a152c5994bd69bf196bda70a6dd2
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09012450B2

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