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Methanol → 3-(2-Methoxyethoxy)azetidine hydrochloride

HRID 2172046
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HRID 2172046 반응식
[Cl:1]C(OC(Cl)C)=O.C([N:21]1[CH2:24][CH:23]([O:25][CH2:26][CH2:27][O:28][CH3:29])[CH2:22]1)(C1C=CC=CC=1)C1C=CC=CC=1.CO>ClCCCl>[ClH:1].[CH3:29][O:28][CH2:27][CH2:26][O:25][CH:23]1[CH2:24][NH:21][CH2:22]1
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참가 물질

5

반응물 3

HCID 887MethanolHCID 5213051-Chloroethyl chloroformateHCID 671545481-Benzhydryl-3-(2-methoxyethoxy)-azetidine

생성물 1

HCID 178173733-(2-Methoxyethoxy)azetidine hydrochloride수율 92.9%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

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온도
70 °C
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실험 절차

1-Chloroethyl chloroformate (102 μL, 0.9 mmol) was added to a solution of 1-benzhydryl-3-(2-methoxyethoxy)-azetidine (215 mg, 0.7 mmol) in 1,2-dichloroethane (3 mL) at room temperature. The reaction mixture was then heated up to 70° C. and stirred for 2.5 hours. After cooling down to room temperature, methanol (3 mL) was added and the reaction mixture was stirred overnight at 70° C. The mixture was then concentrated to dryness and the residue was triturated in pentane (2×15 mL) to give a yellow oil (109 mg, 90%) which was used in the next step without further purification.

후처리

  1. temperatureAfter cooling down to room temperature
  2. stirringthe reaction mixture was stirred overnight at 70° C
  3. concentrationThe mixture was then concentrated to dryness
  4. customthe residue was triturated in pentane (2×15 mL)

출처 및 근거

ORD 기록
ord-0d385ce95fcf4e55a2b40ef6546ca58f
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09051321B2

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