1-Chloroethyl chloroformate → Methyl 2,3-dihydro-1H-isoindole-4-carboxylate--hydrogen chloride (1/1)

HRID 1826996노트

반응식

HRID 1826996 반응식
[CH3:1][O:2][C:3]([C:5]1[C:6]2[CH2:7][N:8](CC3C=CC=CC=3)[CH2:9][C:10]=2[CH:11]=[CH:12][CH:13]=1)=[O:4].[Cl:21]C(OC(Cl)C)=O>ClCCl>[ClH:21].[CH3:1][O:2][C:3]([C:5]1[C:6]2[CH2:7][NH:8][CH2:9][C:10]=2[CH:11]=[CH:12][CH:13]=1)=[O:4]

참가 물질

4

반응물 2

HCID 5213051-Chloroethyl chloroformateHCID 19828480Methyl 2-benzylisoindoline-4-carboxylate

생성물 1

HCID 19828511Methyl 2,3-dihydro-1H-isoindole-4-carboxylate--hydrogen chloride (1/1)

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-10 °C

실험 절차

To a solution of 2-benzyl-2,3-dihydro-1H-isoindole-4-carboxylic acid methyl ester (0.3 g, 1.12 mmol) in dichloromethane (4 ml) at −10° C., was added dropwise α-chloroethyl chloroformate (0.16 ml, 1.46 mmol) and stirred at −10° C. for 30 mins. The solvent was removed by evaporation under reduced pressure and the residue dissolved in methanol (5 ml) and heated to 90° C. for 40 mins. The solution was cooled to room temperature and the solvent removed by evaporation under reduced pressure. The residue was diluted with ethyl acetate (30 ml), extracted into sat. NaOH solution to give a hygroscopic solid, used without further purification.

후처리

  1. customThe solvent was removed by evaporation under reduced pressure
  2. dissolutionthe residue dissolved in methanol (5 ml)
  3. temperatureheated to 90° C. for 40 mins
  4. temperatureThe solution was cooled to room temperature
  5. customthe solvent removed by evaporation under reduced pressure
  6. additionThe residue was diluted with ethyl acetate (30 ml)
  7. extractionextracted into sat. NaOH solution
  8. customto give a hygroscopic solid
  9. customused without further purification

출처 및 근거

ORD 기록
ord-3fb2d936563a4b9095f5ce5b3f2dcfd0
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07053122B2

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