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Hydrochloric Acid → HCID 52914395、化合物

HRID 2177675
ノート
印刷プレビュー

反応式

HRID 2177675 の反応式
[ClH:1].[C:2]1([S:8]([CH2:11][C:12]2[C:17]([C:18]([OH:20])=[O:19])=[C:16]([O:21][CH2:22][CH2:23][NH:24]C(OC(C)(C)C)=O)[C:15]([C:32]3[CH:36]=[CH:35][O:34][CH:33]=3)=[CH:14][CH:13]=2)(=[O:10])=[O:9])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>O1CCOCC1>[ClH:1].[NH2:24][CH2:23][CH2:22][O:21][C:16]1[C:15]([C:32]2[CH:36]=[CH:35][O:34][CH:33]=2)=[CH:14][CH:13]=[C:12]([CH2:11][S:8]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)(=[O:10])=[O:9])[C:17]=1[C:18]([OH:20])=[O:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 671076826-(Benzenesulphonylmethyl)-2-[2-(t-butoxycarbonyl)aminoethoxy]-3-(furan-3-yl)benzoic acid2 回

生成物 1

HCID 52914395HCID 52914395、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Hydrogen chloride (4M in dioxane, 2 ml) was added to a solution of 6-(benzenesulphonylmethyl)-2-[2-(t-butoxycarbonyl)aminoethoxy]-3-(furan-3-yl)benzoic acid (Intermediate 6, 0.018 g) in dioxane (0.5 ml) and the resultant mixture was stirred at room temperature for 2 hours. The mixture was evaporated to dryness and the residue was triturated with ether. The solid was collected by filtration then purified by chromatography on silica, eluting with a mixture of DCM, methanol, acetic acid and water in a ratio of 240:20:3:2 changing to 120:15:3:2. After evaporation of the solvent, the residue was treated with hydrochloric acid (1M) and evaporated to dryness to give 2-(2-aminoethoxy)-6-(benzenesulphonylmethyl)-3-(furan-3-yl)benzoic acid hydrochloride (0.008 g) as a white solid.

後処理

  1. customThe mixture was evaporated to dryness
  2. customthe residue was triturated with ether
  3. filtrationThe solid was collected by filtration
  4. customthen purified by chromatography on silica
  5. washeluting with a mixture of DCM, methanol, acetic acid and water in a ratio of 240:20:3:2 changing to 120:15:3:2
  6. customAfter evaporation of the solvent
  7. additionthe residue was treated with hydrochloric acid (1M)
  8. customevaporated to dryness

出典と根拠

ORDレコード
ord-2c6b655937a04475acc0b399673385bd
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09067905B2

反応ノート

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