Methanesulfonyl chloride → Methyl 3-(cyclopropylmethoxy)-4-(methylsulfonamido)benzoate

HRID 2172584ノート

反応式

HRID 2172584 の反応式
[CH:1]1([CH2:4][O:5][C:6]2[CH:7]=[C:8]([CH:13]=[CH:14][C:15]=2[NH2:16])[C:9]([O:11][CH3:12])=[O:10])[CH2:3][CH2:2]1.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>N1C=CC=CC=1>[CH3:12][O:11][C:9](=[O:10])[C:8]1[CH:13]=[CH:14][C:15]([NH:16][S:18]([CH3:17])(=[O:20])=[O:19])=[C:6]([O:5][CH2:4][CH:1]2[CH2:3][CH2:2]2)[CH:7]=1

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 43560608HCID 43560608、化合物

生成物 1

HCID 59443764Methyl 3-(cyclopropylmethoxy)-4-(methylsulfonamido)benzoate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Methyl 3-(cyclopropylmethoxy)-4-aminobenzoate (8.86 g) was dissolved in pyridine (80 mL) at room temperature under N2 atmosphere. Methanesulfonyl chloride (4.04 mL) was added and the mixture was stirred at r.t. for 18 hours. The reaction mixture was evaporated to dryness, the crude was treated with 1N HCl (500 mL) and extracted with CH2Cl2 (3×200 mL). The organic layer was dried over Na2SO4 and the solvent was evaporated off to yield 11.7 g of the desired intermediate.

後処理

  1. customThe reaction mixture was evaporated to dryness
  2. additionthe crude was treated with 1N HCl (500 mL)
  3. extractionextracted with CH2Cl2 (3×200 mL)
  4. dry with materialThe organic layer was dried over Na2SO4
  5. customthe solvent was evaporated off

出典と根拠

ORDレコード
ord-f617f07ebd9d40aea3c63ee5ced78d93
出典データセット
uspto-grants-2015_06
特許番号
US09056176B2

反応ノート

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