Sulfuric Acid → HCID 66712989、化合物

HRID 250328ノート

反応式

HRID 250328 の反応式
[O:1]=[C:2]1[C:10]2[C:5](=[CH:6][C:7]([S:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[CH:8][CH:9]=2)[C:4](=[O:18])[N:3]1[CH2:19][C:20]([OH:22])=[O:21].S(=O)(=O)(O)O.[C:28](=O)(O)[O-].[Na+]>CO>[CH3:28][O:21][C:20](=[O:22])[CH2:19][N:3]1[C:4](=[O:18])[C:5]2[C:10](=[CH:9][CH:8]=[C:7]([S:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH:6]=2)[C:2]1=[O:1]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 59645281(1,3-Dioxo-5-phenylsulfanyl-1,3-dihydro-isoindol-2-yl)-acetic acid

生成物 1

HCID 66712989HCID 66712989、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 20 ml of methanol, 6.27 g of (1,3-dioxo-5-phenylsulfanyl-1,3-dihydro-isoindol-2-yl)-acetic acid (20 mmol) and 0.3 ml of concentrated sulfuric acid was refluxed with stirring for 18 h. Then 100 ml of concentrated aqueous sodium bicarbonate solution were added and the mixture was extracted with 100 ml of ethyl acetate. The organic phase was dried over MgSO4 and evaporated in vacuo. 6.30 g of the title compound were obtained; MS-(+)-ion: M+1=328.0; 1H NMR (CDCl3): δ=7.69 (d, 1H), 7.41 to 7.55 (m, 7H), 4.40 (s, 2H), 3.75 (s, 3H).

後処理

  1. temperaturewas refluxed
  2. extractionthe mixture was extracted with 100 ml of ethyl acetate
  3. dry with materialThe organic phase was dried over MgSO4
  4. customevaporated in vacuo

出典と根拠

ORDレコード
ord-3546c07ce8324e9e94830531e4f8d89f
出典データセット
uspto-grants-2011_01
特許番号
US07863292B2

反応ノート

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