Acetyl chloride → 7-Acetyl-4-methoxybenzo[d]thiazol-2(3H)-one

HRID 749238ノート

反応式

HRID 749238 の反応式
[CH3:1][O:2][C:3]1[C:8]2[NH:9][C:10](=[O:12])[S:11][C:7]=2[CH:6]=[CH:5][CH:4]=1.[C:13](Cl)(=[O:15])[CH3:14].[Cl-].[Al+3].[Cl-].[Cl-]>ClCCl>[C:13]([C:6]1[C:7]2[S:11][C:10](=[O:12])[NH:9][C:8]=2[C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)(=[O:15])[CH3:14]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 127708784-Methoxy-2(3H)-benzothiazolone

生成物 1

HCID 450769887-Acetyl-4-methoxybenzo[d]thiazol-2(3H)-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 4-methoxy-1,3-benzothiazol-2(3H)-one (DE 3017977 A1) (1.92 g) in dry dichloromethane (50 ml) was cooled to ˜5° C. under nitrogen. Acetyl chloride (1.43 ml) and aluminium chloride (3.43 g) were added in one portion, and stirred for 2 h at RT. The reaction was quenched carefully with water, followed by addition of 2N HCl and dichloromethane. The aqueous layer was extracted with dichloromethane, and the combined organic layers were washed with brine and dried (Na2SO4) and evaporated in vacuo to give the title compound (1.92 g). LCMS RT=2.50 min

後処理

  1. customThe reaction was quenched carefully with water
  2. additionfollowed by addition of 2N HCl and dichloromethane
  3. extractionThe aqueous layer was extracted with dichloromethane
  4. washthe combined organic layers were washed with brine
  5. dry with materialdried (Na2SO4)
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-8ac670beee6d43589a1fc5b855c60a6b
出典データセット
uspto-grants-2008_07
特許番号
US07402598B2

反応ノート

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