Hydrochloric Acid → HCID 12098836, 화합물

HRID 989458노트

반응식

HRID 989458 반응식
C([Li])CCC.[CH2:6]([Cl:8])[Cl:7].[CH2:9]([N:16]([CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C@H:17]([C:25](O)=[O:26])[CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.Cl>CCCCCC.O1CCCC1.O>[Cl:7][CH:6]([Cl:8])[C:25](=[O:26])[C@@H:17]([N:16]([CH2:9][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)[CH2:28][C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1)[CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 10980880N,N-Dibenzyl-L-phenylalanineHCID 178418339Butyllithium

생성물 1

HCID 12098836HCID 12098836, 화합물수율 99%

시약·촉매·용매 3

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매3회HCID 8058Hexane용매

실험 절차

Dehydrated tetrahydrofuran (15 ml) was cooled to −78° C. 1.53 M solution (6.5 ml) of n-butyllithium in hexane and then a solution of methylene chloride (0.8 ml) in dehydrated tetrahydrofuran (5 ml) were added thereto, and they were stirred for 10 minutes. A solution of benzyl ester (2.18 g) of N,N-dibenzyl-L-phenylalanine in dehydrated tetrahydrofuran (7 ml) was added to the obtained mixture, and they were stirred for 1 hour. 2 N hydrochloric acid (15 ml) and water (15 ml) were added to the reaction mixture to terminate the reaction. The temperature was elevated to room temperature. After the addition of water followed by the extraction with ethyl acetate, the obtained solutions in ethyl acetate were combined together and dried over anhydrous magnesium sulfate. Magnesium sulfate was filtered out. The solvent was evaporated under reduced pressure to obtain the intended (3S)-1,1-dichloro-3-dibenzylamino-4-phenyl-2-butanone (2.04 g) in a yield of 99%.

후처리

  1. stirringwere stirred for 1 hour
  2. customto terminate
  3. customthe reaction
  4. customwas elevated to room temperature
  5. extractionfollowed by the extraction with ethyl acetate
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationMagnesium sulfate was filtered out
  8. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-f2421b823cac4d0cb2570336223206b1
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06639094B2

반응 노트

불러오는 중…