Boron trifluoride etherate → HCID 86615014, 화합물

HRID 1436683노트

반응식

HRID 1436683 반응식
B(F)(F)F.CCOCC.[CH3:10][O:11][C:12](=[O:34])[C:13]1[CH:25]=[C:24]([C:26](=O)[C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH:23]=[C:15]([C:16]([N:18]([CH3:22])[CH2:19][CH2:20][CH3:21])=[O:17])[CH:14]=1.[CH2:35]([SH:39])[CH2:36][CH2:37][SH:38]>ClCCl>[CH3:10][O:11][C:12](=[O:34])[C:13]1[CH:25]=[C:24]([C:26]2([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[S:39][CH2:35][CH2:36][CH2:37][S:38]2)[CH:23]=[C:15]([C:16]([N:18]([CH3:22])[CH2:19][CH2:20][CH3:21])=[O:17])[CH:14]=1

참가 물질

5

반응물 3

HCID 8000Boron trifluoride etherateHCID 80131,3-PropanedithiolHCID 68814475HCID 68814475, 화합물

생성물 1

HCID 86615014HCID 86615014, 화합물수율 51%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Add boron trifluoride diethyl etherate (0.358 mL, 2.83 mmol) to a solution of 5-benzoyl-N-methyl-N-propyl-isophthalamic acid methyl ester (0.192 g, 0.566 mmol) in dichloromethane (3 mL) at 0° C. Add 1,3-propanedithiol (0.114 mL, 1.12 mmol). Stir at room temperature overnight. Partition between water (20 mL) and dichloromethane (20 mL) and extract the aqueous layer with dichloromethane (20 mL). Dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 30:70 ethyl acetate:hexanes) to give the title compound (51%).

후처리

  1. customPartition between water (20 mL) and dichloromethane (20 mL)
  2. extractionextract the aqueous layer with dichloromethane (20 mL)
  3. dry with materialDry (magnesium sulfate)
  4. concentrationconcentrate
  5. custompurify
  6. wash(silica gel chromatography, eluting with 30:70 ethyl acetate:hexanes)

출처 및 근거

ORD 기록
ord-7a375fd892a14dfb8400bd4f1f7486c5
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618978B2

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