Hydrochloric Acid → HCID 12098836、化合物

HRID 989458ノート

反応式

HRID 989458 の反応式
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

参加物

8

反応物 4

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

生成物 1

HCID 12098836HCID 12098836、化合物収率 99%

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒3 回HCID 8058Hexane溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-f2421b823cac4d0cb2570336223206b1
出典データセット
uspto-grants-2003_10
特許番号
US06639094B2

反応ノート

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