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Acetic Acid → (S)-3-[1-(4,6-dimethyl-benzo[d]isothiazol-3-ylmethyl)-2,4-dioxo-1,4-dihydro-2H-pyrido[3,2-d]pyrimidin-3-yl]-pentanoic acid

HRID 1887194
ノート
印刷プレビュー

反応式

HRID 1887194 の反応式
C[O:2][C:3](=[O:32])[CH2:4][C@@H:5]([N:8]1[C:13](=[O:14])[C:12]2[N:15]=[CH:16][CH:17]=[CH:18][C:11]=2[N:10]([CH2:19][C:20]2[C:24]3[C:25]([CH3:30])=[CH:26][C:27]([CH3:29])=[CH:28][C:23]=3[S:22][N:21]=2)[C:9]1=[O:31])[CH2:6][CH3:7].[OH-].[Li+].C(O)(=O)C.O>O1CCOCC1>[CH3:30][C:25]1[C:24]2[C:20]([CH2:19][N:10]3[C:11]4[CH:18]=[CH:17][CH:16]=[N:15][C:12]=4[C:13](=[O:14])[N:8]([C@@H:5]([CH2:6][CH3:7])[CH2:4][C:3]([OH:32])=[O:2])[C:9]3=[O:31])=[N:21][S:22][C:23]=2[CH:28]=[C:27]([CH3:29])[CH:26]=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 176Acetic AcidHCID 962WaterHCID 3939Lithium HydroxideHCID 67503561(S)-3-[1-(4,6-dimethyl-benzo[d]isothiazol-3-ylmethyl)-2,4-dioxo-1,4-dihydro-2H-pyrido[3,2-d]pyrimidin-3-yl]-pentanoic acid methyl ester

生成物 1

HCID 46853666(S)-3-[1-(4,6-dimethyl-benzo[d]isothiazol-3-ylmethyl)-2,4-dioxo-1,4-dihydro-2H-pyrido[3,2-d]pyrimidin-3-yl]-pentanoic acid収率 34%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 80 mg of (S)-3-[1-(4,6-dimethyl-benzo[d]isothiazol-3-ylmethyl)-2,4-dioxo-1,4-dihydro-2H-pyrido[3,2-d]pyrimidin-3-yl]-pentanoic acid methyl ester in 1,4-dioxane (2.5 mL) is added lithium hydroxide solution (11 mg of lithium hydroxide monohydrate in 0.5 mL of water) at room temperature. The solution is stirred at the same temperature for 3.5 h. Then 0.5 mL of acetic acid is added along with 25 mL of water. The mixture is extracted with ethyl acetate (3×50 mL). The combined organic layers are dried over sodium sulfate and concentrated. The residue is purified by flash chromatography on silica gel to give 26 mg (34%) of (S)-3-[1-(4,6-dimethyl-benzo[d]isothiazol-3-ylmethyl)-2,4-dioxo-1,4-dihydro-2H-pyrido[3,2-d]pyrimidin-3-yl]-pentanoic acid; LCMS (ESMS): m/z 439.12 (M+H+).

後処理

  1. extractionThe mixture is extracted with ethyl acetate (3×50 mL)
  2. dry with materialThe combined organic layers are dried over sodium sulfate
  3. concentrationconcentrated
  4. customThe residue is purified by flash chromatography on silica gel

出典と根拠

ORDレコード
ord-63c25d5536534924aa3eae3a9ebfd9fe
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08501749B2

反応ノート

読み込み中…

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