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Sodium Hydroxide → HCID 19004497、化合物

HRID 2225809
ノート
印刷プレビュー

反応式

HRID 2225809 の反応式
C[O:2][C:3](=[O:25])[C:4](=[O:24])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][C:13]([NH:15][CH:16]2[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)=[O:14])=[CH:7][CH:6]=1.[OH-].[Na+]>CO>[CH:16]1([NH:15][C:13](=[O:14])[CH2:12][O:11][C:8]2[CH:7]=[CH:6][C:5]([C:4](=[O:24])[C:3]([OH:25])=[O:2])=[CH:10][CH:9]=2)[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]1
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 14798Sodium HydroxideHCID 54288573HCID 54288573、化合物

生成物 1

HCID 19004497HCID 19004497、化合物収率 21.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 4-[2-(cyclooctylamino)-2-oxoethoxy]-alpha-oxobenzeneacetic acid methyl ester (0.4 g) in methanol (40 mL) was treated with 1N sodium hydroxide solution (1.3 mL), and the mixture was stirred at room temperature for 15 minutes. After the solvents were evaporated under reduced pressure, water (20 mL) was added and the solution was acidified with 3N hydrochloric acid, then the aqueous layer was extracted with a mixture of dichloromethane-tetrahydrofuran (30 mL; 2:1). The organic layer was dried (MgSO4), evaporated and the resulting oil was crystallized from diethyl ether-hexane to yield 0.084 g of 4-[2-(cyclooctylamino)-2-oxoethoxy]-alpha-oxobenzeneacetic acid, mp 139°-140 ° C.

後処理

  1. customAfter the solvents were evaporated under reduced pressure, water (20 mL)
  2. additionwas added
  3. extractionthe aqueous layer was extracted with a mixture of dichloromethane-tetrahydrofuran (30 mL; 2:1)
  4. dry with materialThe organic layer was dried (MgSO4)
  5. customevaporated
  6. customthe resulting oil was crystallized from diethyl ether-hexane

出典と根拠

ORDレコード
ord-f2f20167ecbc496487137a17998ae789
出典データセット
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05344843

反応ノート

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