Ethanol → HCID 67154553, 화합물

HRID 633938

반응식

HRID 633938 반응식
[Cl:1]C(OC(Cl)=O)C.C([N:21]1[CH2:24][CH:23]([O:25][CH2:26][CH2:27][C:28]2[S:29][CH:30]=[CH:31][CH:32]=2)[CH2:22]1)(C1C=CC=CC=1)C1C=CC=CC=1.C(O)C>ClCCl>[ClH:1].[ClH:1].[S:29]1[CH:30]=[CH:31][CH:32]=[C:28]1[CH2:27][CH2:26][O:25][CH:23]1[CH2:24][NH:21][CH2:22]1

참가 물질

5

반응물 3

HCID 702EthanolHCID 5213051-Chloroethyl chloroformateHCID 671545391-Benzhydryl-3-(2-(thiophen-2-yl)ethoxy)azetidine

생성물 1

HCID 67154553HCID 67154553, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1-Chloroethylchloroformate (361 μL, 3.33 mmol) was added to a solution of 1-benzhydryl-3-(2-(thiophen-2-yl)ethoxy)azetidine (1.11 g, 3.17 mmol) in dichloromethane (15 mL) at room temperature. The reaction mixture was stirred overnight at room temperature, then 1 hour at 70° C. After cooling down to room temperature, ethanol (15 mL) was added and the reaction mixture was stirred at 70° C. for 1 hour. After concentration to dryness, the crude mixture was triturated in pentane (2×15 mL) to give a yellow oil (698 mg, quantitative) which was used in the next step without further purification.

후처리

  1. custom1 hour
  2. customat 70° C
  3. temperatureAfter cooling down to room temperature
  4. stirringthe reaction mixture was stirred at 70° C. for 1 hour
  5. concentrationAfter concentration to dryness
  6. customthe crude mixture was triturated in pentane (2×15 mL)
  7. customto give a yellow oil (698 mg, quantitative) which
  8. customwas used in the next step without further purification

출처 및 근거

ORD 기록
ord-493fa3e3df824bd49a8f8e3cd5759391
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321769B2

연결된 노트

불러오는 중…