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Water → 2-(1,4-Dioxa-8-azaspiro[4.5]decan-8-ylcarbonyl)aminobenzoic Acid

HRID 1373710
ノート
印刷プレビュー

反応式

HRID 1373710 の反応式
[O:1]1[C:5]2([CH2:10][CH2:9][N:8]([C:11]([NH:13][C:14]3[CH:23]=[CH:22][CH:21]=[CH:20][C:15]=3[C:16]([O:18]C)=[O:17])=[O:12])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.[OH-].[Na+].CCOC(C)=O.O>O1CCOCC1>[O:4]1[C:5]2([CH2:6][CH2:7][N:8]([C:11]([NH:13][C:14]3[CH:23]=[CH:22][CH:21]=[CH:20][C:15]=3[C:16]([OH:18])=[O:17])=[O:12])[CH2:9][CH2:10]2)[O:1][CH2:2][CH2:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 17383362Methyl 2-[(1,4-dioxa-8-azaspiro[4.5]dec-8-ylcarbonyl)amino]benzoate

生成物 1

HCID 219062722-(1,4-Dioxa-8-azaspiro[4.5]decan-8-ylcarbonyl)aminobenzoic Acid

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane
溶媒

実験手順

A solution of methyl 2-(1,4-dioxa-8-azaspiro[4.5]decan-8-ylcarbonyl)aminobenzoate (2.00 g, 6.25 mmol) in dioxane (30 mL) was treated with 5 N NaOH (12.5 mL). After 1 h, the mixture was poured into EtOAc and water, and the aqueous layer was washed with EtOAc. The pH of the aqueous layer was then adjusted to 2–3 by addition of 5 N HCl and washed with EtOAc (3×). The combined organic layers were washed with brine, dried with sodium sulfate, and concentrated, yielding the title compound; which was used without further purification.

後処理

  1. washthe aqueous layer was washed with EtOAc
  2. additionThe pH of the aqueous layer was then adjusted to 2–3 by addition of 5 N HCl
  3. washwashed with EtOAc (3×)
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried with sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-3e8d43113439431e8adebae8c56c3721
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07163938B2

反応ノート

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