Nitrogen → 4-Chloromethyl-thiazole-2-carbaldehyde

HRID 42794

反応式

HRID 42794 の反応式
N#N.[Cl:3][CH2:4][C:5]1[N:6]=[C:7]([CH2:10][OH:11])[S:8][CH:9]=1>C(C#N)(C)=O.O=[Mn]=O>[Cl:3][CH2:4][C:5]1[N:6]=[C:7]([CH:10]=[O:11])[S:8][CH:9]=1

参加物

5

反応物 2

HCID 947NitrogenHCID 11073749[4-(Chloromethyl)-1,3-thiazol-2-yl]methanol

生成物 1

HCID 552985444-Chloromethyl-thiazole-2-carbaldehyde

試薬・触媒・溶媒 2

HCID 14801Manganese dioxide触媒HCID 694302-Oxopropiononitrile溶媒

実験手順

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of (4-chloromethyl-thiazol-2-yl)-methanol (1.60 g, 9.80 mmol) in AcCN (98.0 mL) was treated at rt with MnO2 (4.73 g, 49.01 mmol). The reaction mixture was stirred at rt overnight before being filtered through Celite and the solvent was removed under reduced pressure. Purification of the residue by FC (4:1 hept-EA) gave the title compound as a colorless oil. TLC:rf (4:1 hept-EA)=0.37. LC-MS-conditions 02: tR=0.77 min.

後処理

  1. filtrationbefore being filtered through Celite
  2. customthe solvent was removed under reduced pressure
  3. customPurification of the residue by FC (4:1 hept-EA)

出典と根拠

ORDレコード
ord-7a7c569c4fa34f09b0e58e1a59c58918
出典データセット
uspto-grants-2013_09
特許番号
US08536209B2

関連ノート

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