Iodine → Bis(thiobenzoyl) Disulfide

HRID 1636033ノート

反応式

HRID 1636033 の反応式
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

参加物

4

反応物 2

HCID 807IodineHCID 11030352Sodium dithiobenzoate

生成物 1

HCID 10902862Bis(thiobenzoyl) Disulfide収率 50%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-0b904497e7494475b98f17c298a9f463
出典データセット
uspto-grants-2003_01
特許番号
US06512081B1

反応ノート

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