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Hydrochloric Acid → 4-(1-Benzyloxycarbonylaminocyclopropyl)-2,3,5,6tetrafluorobenzoic acid

HRID 981274
ノート
印刷プレビュー

反応式

HRID 981274 の反応式
[CH2:1]([O:8][C:9]([NH:11][C:12]1([C:15]2[C:24]([F:25])=[C:23]([F:26])[C:18]([C:19]([O:21]C)=[O:20])=[C:17]([F:27])[C:16]=2[F:28])[CH2:14][CH2:13]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].O.Cl>CO.O1CCOCC1.C(OCC)(=O)C>[CH2:1]([O:8][C:9]([NH:11][C:12]1([C:15]2[C:16]([F:28])=[C:17]([F:27])[C:18]([C:19]([OH:21])=[O:20])=[C:23]([F:26])[C:24]=2[F:25])[CH2:13][CH2:14]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 15136259Methyl 4-(1-benzyloxycarbonylaminocyclopropyl)-2,3,5,6-tetrafluorobenzoate

生成物 1

HCID 100454814-(1-Benzyloxycarbonylaminocyclopropyl)-2,3,5,6tetrafluorobenzoic acid収率 97.9%

試薬・触媒・溶媒 3

HCID 887
Methanol
溶媒
HCID 8857Ethyl Acetate溶媒
HCID 312751,4-Dioxane溶媒

実験手順

In a mixture of 14 ml of methanol and 14 ml of dioxane was dissolved 1.8 g of methyl 4-(1-benzyloxycarbonylaminocyclopropyl)-2,3,5,6-tetrafluorobenzoate. To the resulting solution was added 14 ml of a 1N aqueous sodium hydroxide solution. The resulting mixture was stirred at room temperature for 1 hour. To the reaction mixture was added 50 ml of water. The resulting mixture was adjusted to pH 1 with 2N hydrochloric acid, and 50 ml of ethyl acetate was added thereto. The organic layer was separated, washed with water and a saturated aqueous sodium chloride solution in this order, and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure, and n-hexane was added to the residue obtained. The resulting crystals were collected by filtration to obtain 1.7 g (yield: 97.7%) of 4-(1-benzyloxycarbonylaminocyclopropyl)-2,3,5,6tetrafluorobenzoic acid.

後処理

  1. additionwas added
  2. customThe organic layer was separated
  3. washwashed with water
  4. dry with materiala saturated aqueous sodium chloride solution in this order, and dried over anhydrous magnesium sulfate
  5. customThe solvent was removed by distillation under reduced pressure, and n-hexane
  6. additionwas added to the residue
  7. customobtained
  8. filtrationThe resulting crystals were collected by filtration

出典と根拠

ORDレコード
ord-8742601296844af4835a876469d549af
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04990508

反応ノート

読み込み中…

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