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Hydrochloric Acid → HCID 53636182、化合物

HRID 24667
ノート
印刷プレビュー

反応式

HRID 24667 の反応式
[CH3:1][O:2][C:3](=[O:37])[C@H:4]([CH2:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[C:28]([O:29][CH3:30])=[CH:27][CH:26]=[C:25]([O:31]COC)[C:24]=2[O:35][CH3:36])=[CH:19][CH:18]=1)[NH:5][C:6](=[O:15])[C:7]1[C:12]([Cl:13])=[CH:11][CH:10]=[CH:9][C:8]=1[Cl:14].Cl>CO.O1CCOCC1>[CH3:1][O:2][C:3](=[O:37])[C@H:4]([CH2:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[C:28]([O:29][CH3:30])=[CH:27][CH:26]=[C:25]([OH:31])[C:24]=2[O:35][CH3:36])=[CH:19][CH:18]=1)[NH:5][C:6](=[O:15])[C:7]1[C:12]([Cl:13])=[CH:11][CH:10]=[CH:9][C:8]=1[Cl:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 53989823HCID 53989823、化合物

生成物 1

HCID 53636182HCID 53636182、化合物収率 95.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

N-(2,6-Dichlorobenzoyl)-4-(2,6-dimethoxy-3-methoxymethoxyphenyl)-L-phenylalanine methyl ester (165 mg) was dissolved in MeOH (5 mL) and HCl in dioxane (4 M, 1 mL) was added to the mixture. The mixture was stirred at room temperature for 3 h. The mixture was evaporated and the residue was taken up with water (40 mL) and extracted with CH2Cl2. The extract was dried (MgSO4), filtered and evaporated. The residue was purified by preparative TLC (silica gel; eluent: hexane and AcOEt 3:1 to 1:1) to give N-(2,6-dichlorobenzoyl)-4-(2,6-dimethoxy-3-hydroxyphenyl)-L-phenylalanine methyl ester (145 mg).

後処理

  1. customThe mixture was evaporated
  2. extractionextracted with CH2Cl2
  3. dry with materialThe extract was dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was purified by preparative TLC (silica gel; eluent: hexane and AcOEt 3:1 to 1:1)

出典と根拠

ORDレコード
ord-4d3b5633c42c456c875af73074e4b486
出典データセット
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06855843B2

反応ノート

読み込み中…

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