Sulfuric Acid → HCID 66712989, 화합물

HRID 1406091노트

반응식

HRID 1406091 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 66712989HCID 66712989, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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, 1 H), 7.41 to 7.55 (m, 7 H), 4.40 (s, 2 H), 3.75 (s, 3 H).

후처리

  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

출처 및 근거

ORD 기록
ord-217d22b3fca342b1a639d2bed934b727
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08916585B2

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