1,2-Dichloroethane → 3-[(2-Methylprop-2-en-1-yl)oxy]azetidine hydrochloride

HRID 633906

반응식

HRID 633906 반응식
C1(C(C2C=CC=CC=2)[N:8]2[CH2:11][CH:10]([O:12][CH2:13][C:14]([CH3:16])=[CH2:15])[CH2:9]2)C=CC=CC=1.[Cl:23]CCCl.ClC(OC(Cl)C)=O>CO>[ClH:23].[CH3:16][C:14](=[CH2:15])[CH2:13][O:12][CH:10]1[CH2:11][NH:8][CH2:9]1

참가 물질

5

반응물 3

HCID 111,2-DichloroethaneHCID 5213051-Chloroethyl chloroformateHCID 671545541-(Diphenylmethyl)-3-[(2-methylprop-2-en-1-yl)oxy]azetidine

생성물 1

HCID 671544963-[(2-Methylprop-2-en-1-yl)oxy]azetidine hydrochloride

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
70 °C

실험 절차

A 16 mL flask was charged with 1-(diphenylmethyl)-3-[(2-methylprop-2-en-1-yl)oxy]azetidine (276 mg, 0.94 mmol; which may be prepared as described in Step 1) and 1,2-dichloroethane (4.1 mL). 1-Chloroethyl chloroformate (135 μL, 1.24 mmol) was added and the reaction mixture was stirred at 70° C. for 1.5 h. After cooling to room temperature, methanol (4.1 mL) was added and the reaction mixture was stirred at 70° C. for 1.5 h. The reaction mixture was concentrated to dryness and the residue was triturated in pentane to give the final product (192 mg, quantitative) as a brown oil.

후처리

  1. temperatureAfter cooling to room temperature
  2. stirringthe reaction mixture was stirred at 70° C. for 1.5 h
  3. concentrationThe reaction mixture was concentrated to dryness
  4. customthe residue was triturated in pentane

출처 및 근거

ORD 기록
ord-1dc1f4c2bb73409aaa72791695f25fbe
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321769B2

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