(3-Chloro-5,6-dimethoxy-benzo[b]thiophen-2-yl)methanol → 3-Chloro-5,6-dimethoxy-benzo[b]thiophene-2-carbaldehyde

HRID 1004115ノート

反応式

HRID 1004115 の反応式
[Cl:1][C:2]1[C:3]2[CH:12]=[C:11]([O:13][CH3:14])[C:10]([O:15][CH3:16])=[CH:9][C:4]=2[S:5][C:6]=1[CH2:7][OH:8]>C1(C)C=CC=CC=1.O=[Mn]=O>[Cl:1][C:2]1[C:3]2[CH:12]=[C:11]([O:13][CH3:14])[C:10]([O:15][CH3:16])=[CH:9][C:4]=2[S:5][C:6]=1[CH:7]=[O:8]

参加物

4

反応物 1

HCID 10956261(3-Chloro-5,6-dimethoxy-benzo[b]thiophen-2-yl)methanol

生成物 1

HCID 117801503-Chloro-5,6-dimethoxy-benzo[b]thiophene-2-carbaldehyde

試薬・触媒・溶媒 2

HCID 14801Manganese dioxide触媒3 回HCID 1140Toluene溶媒

実験手順

96 mmol (1.6 equivalents) of MnO2 are added at room temperature under an inert atmosphere to a suspension of 60.4 mmol of the compound obtained in Step C in 360 ml of toluene. After 6 hours' reaction at 80° C., 0.6 equivalent of MnO2 is added to the reaction mixture, followed six hours later by 0.6 equivalent of MnO2. The reaction mixture is then filtered while hot over Celite and rinsed with toluene. After 12 hours at room temperature, the filtrate precipitates. Filtration of the precipitate followed by rinsing with toluene and then with pentane enables 8.65 g of the expected product to be isolated.

後処理

  1. customAfter 6 hours' reaction at 80° C.
  2. filtrationThe reaction mixture is then filtered while hot over Celite
  3. washrinsed with toluene
  4. customthe filtrate precipitates
  5. filtrationFiltration of the precipitate
  6. washby rinsing with toluene
  7. customto be isolated

出典と根拠

ORDレコード
ord-4fa270bd9fc647eead3cdabb8f362ef4
出典データセット
uspto-grants-2000_04
特許番号
US06048875

反応ノート

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