Chlorotrimethylsilane → Dimethyl 3,3'-(((3-formylphenyl)methylene)bis(sulfanediyl))dipropanoate

HRID 22586

反応式

HRID 22586 の反応式
[CH:1](=O)[C:2]1[CH:9]=[CH:8][CH:7]=[C:4]([CH:5]=[O:6])[CH:3]=1.[SH:11][CH2:12][CH2:13][C:14]([O:16][CH3:17])=[O:15].C[Si](Cl)(C)C>C(Cl)(Cl)Cl>[CH:5]([C:4]1[CH:3]=[C:2]([CH:1]([S:11][CH2:12][CH2:13][C:14]([O:16][CH3:17])=[O:15])[S:11][CH2:12][CH2:13][C:14]([O:16][CH3:17])=[O:15])[CH:9]=[CH:8][CH:7]=1)=[O:6]

参加物

5

反応物 3

HCID 6397ChlorotrimethylsilaneHCID 18050Methyl 3-mercaptopropionateHCID 34777Isophthalaldehyde

生成物 1

HCID 10021188Dimethyl 3,3'-(((3-formylphenyl)methylene)bis(sulfanediyl))dipropanoate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a solution of isophthalaldehyde (40 g, 0.3 mol.) in chloroform (400 mL) and methyl 3-mercaptopropanoate (68 mL, 0.6 mol.) was added dropwise trimethylsilyl chloride (48 mL, 0.38 mol.) over 30 min. The reaction mixture was stirred at R.T. for 2 hours. The reaction was quenched with 25% aq. NH4OAc, extracted with ethyl acetate dried and evaporated. Flash chromatography of the residue afforded 50 gl of the title compound.

後処理

  1. customThe reaction was quenched with 25% aq. NH4OAc
  2. extractionextracted with ethyl acetate
  3. customdried
  4. customevaporated

出典と根拠

ORDレコード
ord-92e9c016c1de419ea0a48330884174ff
出典データセット
uspto-grants-1995_06
特許番号
US05428171

関連ノート

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