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Methanol → HCID 22561682、化合物

HRID 1839674
ノート
印刷プレビュー

反応式

HRID 1839674 の反応式
O[O:2][S:3]([O-:5])=O.[K+].C([O:9][C:10]([C:12]1[C:16]([CH2:17][CH2:18][CH2:19]SC)=[C:15]([CH:22]=[O:23])[NH:14][C:13]=1[CH3:24])=[O:11])C.[CH3:25]O>O>[CH:22]([C:15]1[NH:14][C:13]([CH3:24])=[C:12]([C:10]([OH:11])=[O:9])[C:16]=1[CH2:17][CH2:18][CH2:19][S:3]([CH3:25])(=[O:5])=[O:2])=[O:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 20761747HCID 20761747、化合物HCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 22561682HCID 22561682、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

Oxone (614 mg, 1 mmol) dissolved in water (2 mL) was added portionwise to a solution of 5-formyl-2-methyl-4-(3-methylsulfanyl-propyl)-1H-pyrrole-3-carboxylic acid ethyl ester (269 mg, 1 mmol) in methanol (4 mL) cooled in an ice bath. The mixture was stirred for 3 hours, keeping the temp between 0° C. and rt. The reaction was diluted with 10 mL of water, the resulted precipitate was collected by vacuum filtration, washed with water and dried to give 95 mg of the desired product. The water filtrate was extracted with ethyl acetate, dried and concentrated to give another 74 mg of the product. Total of 169 mg (56%) of 5-formyl-4-(3-methanesulfonyl-propyl)-2-methyl-1H-pyrrole-3-carboxylic acid ethyl ester was obtained.

後処理

  1. temperaturecooled in an ice bath
  2. customthe temp between 0° C. and rt
  3. filtrationthe resulted precipitate was collected by vacuum filtration
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-94460a2f39fa4a559194c3da86ce8d4d
出典データセット
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06677368B2

反応ノート

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