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Methanesulfonic Acid → HCID 67458340、化合物

HRID 554819
ノート
印刷プレビュー

反応式

HRID 554819 の反応式
C(O[C:6]([NH:8][CH2:9][C@H:10]([CH2:14][C:15]1[CH:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:16]=1[O:22][CH3:23])[C:11]([OH:13])=[O:12])=O)(C)(C)C.CS(O)(=O)=O.[CH3:29][O:30][C:31]1[CH:38]=[C:37]([O:39][CH3:40])[CH:36]=[C:35]([O:41][CH3:42])[C:32]=1C=O.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[OH-].[Na+]>C(OCC)(=O)C.C(N(CC)CC)C>[Cl:21][C:19]1[CH:18]=[CH:17][C:16]([O:22][CH3:23])=[C:15]([CH:20]=1)[CH2:14][C@@H:10]([CH2:9][NH:8][CH2:6][C:32]1[C:35]([O:41][CH3:42])=[CH:36][C:37]([O:39][CH3:40])=[CH:38][C:31]=1[O:30][CH3:29])[C:11]([OH:13])=[O:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6395Methanesulfonic AcidHCID 14798Sodium HydroxideHCID 700192,4,6-TrimethoxybenzaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 66935162(2S)-3-[(tert-butoxycarbonyl)amino]-2-(5-chloro-2-methoxybenzyl)propanoic acid

生成物 1

HCID 67458340HCID 67458340、化合物

試薬・触媒・溶媒 2

HCID 8471Triethylamine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

(2S)-3-[(tert-butoxycarbonyl)amino]-2-(5-chloro-2-methoxybenzyl)propionic acid (10g) was dissolved in ethyl acetate (120 ml), then methane sulfonic acid (9.4 ml) was added at room temperature, and the resulting mixture was stirred at that temperature for 2 hours. To the reaction solution was added triethylamine (20.3 ml), and the mixture was stirred for 13 hours. Then 2,4,6-trimethoxybenzaldehyde (5.7 g) was added and the mixture was stirred for 30 minutes. Next, to the reaction solution, sodium triacetoxyborohydride (9.3 g) was added and the mixture was stirred for 2 hours. To the reaction solution, a 1N aqueous sodium hydroxide solution was added, and the layers were separated. The aqueous layer was extracted again with ethyl acetate. The organic layer was washed with a 1N aqueous sodium hydroxide solution, then the appeared precipitated crystals were collected by filtration and dried to obtain the title compound (11.5 g) as a colorless crystal.

後処理

  1. stirringthe mixture was stirred for 13 hours
  2. stirringthe mixture was stirred for 30 minutes
  3. stirringthe mixture was stirred for 2 hours
  4. customthe layers were separated
  5. extractionThe aqueous layer was extracted again with ethyl acetate
  6. washThe organic layer was washed with a 1N aqueous sodium hydroxide solution
  7. customthe appeared precipitated crystals
  8. filtrationwere collected by filtration
  9. customdried

出典と根拠

ORDレコード
ord-a936a41559074d77bac253747f5ebdbc
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08049006B2

反応ノート

読み込み中…

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