Iodine → Bis(thiobenzoyl) Disulfide

HRID 1636033

반응식

HRID 1636033 반응식
II.[Na+].[C:4]([S-:12])(=[S:11])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>C(OCC)C>[C:4]([S:12][S:12][C:4](=[S:11])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)(=[S:11])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

참가 물질

4

반응물 2

HCID 807IodineHCID 11030352Sodium dithiobenzoate

생성물 1

HCID 10902862Bis(thiobenzoyl) Disulfide수율 50%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

An aqueous solution of iodine (1.0 N, 100 mL) was added dropwise to a stirred aqueous solution of dithiobenzoic acid sodium salt (0.1 mol in 100 mL of water) at room temperature over 15 minutes. Diethyl ether (100 mL) was added, the organic layer separated and washed twice with water, dried (Na2SO4), filtered and concentrated in vacuo. Di(thiobenzoyl)disulfide (7.5 g, 50%) was obtained after recrystallization from hot ethanol, m.p. 89-91° C. [lit(Houben, Chem, Ber., 39, 3219-3233, (1906). m.p. 92.5° C.]. 1H-nmr (CDCl3) δ (ppm) 7.44 (m, 4H, meta-ArH); 7.62 (m, 2H, para-ArH) and 8.11 (m, 4H, ortho-ArH).

후처리

  1. customthe organic layer separated
  2. washwashed twice with water
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-0b904497e7494475b98f17c298a9f463
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06512081B1

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