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Diisopropylethylamine → 1-[1-(4-Chloro-phenyl)-cyclobutanecarbonyl]-azetidine-3-carboxylic acid methyl ester

HRID 2110298
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HRID 2110298 반응식
Cl.[CH3:2][O:3][C:4]([CH:6]1[CH2:9][NH:8][CH2:7]1)=[O:5].[Cl:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2([C:21](O)=[O:22])[CH2:20][CH2:19][CH2:18]2)=[CH:13][CH:12]=1.C(N(C(C)C)CC)(C)C.C1CN([P+](Br)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F>C(Cl)Cl>[CH3:2][O:3][C:4]([CH:6]1[CH2:9][N:8]([C:21]([C:17]2([C:14]3[CH:13]=[CH:12][C:11]([Cl:10])=[CH:16][CH:15]=3)[CH2:18][CH2:19][CH2:20]2)=[O:22])[CH2:7]1)=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 6027611-(p-Chlorophenyl)cyclobutanecarboxylic acidHCID 2733179PyBroPHCID 21100040Methyl azetidine-3-carboxylate hydrochloride

생성물 1

HCID 587375011-[1-(4-Chloro-phenyl)-cyclobutanecarbonyl]-azetidine-3-carboxylic acid methyl ester수율 70.6%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

To a stirred solution of azetidine-3-carboxylic acid methyl ester hydrochloride (762 mg, 4.60 mmoles) and 1-(4-chloro-phenyl)-cyclobutane carboxylic acid (2.09 g, 9.90 mmoles) in anhydrous DCM (20 mL) was added di-isopropyl ethyl amine (4.6 mL, 26.4 mmoles) dropwise. After completion of addition solid PyBroP (4.63 g, 9.94 mmoles) was added to the stirring reaction mixture. The reaction mixture continued stirring at RT for 10 h and was quenched with water. The aqueous layer was extracted with EtOAc (3×20 mL). Combined organic layers were dried over Na2SO4 and concentrated to yield an oil. This crude material was purified using silica gel chromatography (9:1 hexanes:EtOAc-1:1 hexane:EtOAc) to yield the desired amide (1.0 g, 65%). 1H NMR (300 MHz, CDCl3): δ 7.38-7.29 (m, 4H), 4.16 (m, 2H), 3.88 (m, 1H), 3.72 (s, 3H), 3.31-1.63 (m, 8H). LRMS: M+309.

후처리

  1. additionwas added to the stirring reaction mixture
  2. customwas quenched with water
  3. extractionThe aqueous layer was extracted with EtOAc (3×20 mL)
  4. dry with materialCombined organic layers were dried over Na2SO4
  5. concentrationconcentrated
  6. customto yield an oil
  7. customThis crude material was purified

출처 및 근거

ORD 기록
ord-2259dd80b002452297d354e754db6ee2
출처 데이터셋
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07517892B2

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