Hydrochloric Acid → HCID 65751811、化合物

HRID 1669359ノート

反応式

HRID 1669359 の反応式
[CH3:1][O:2][CH2:3][CH2:4][NH:5][S:6]([C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[C:12](O)=[O:13])(=[O:8])=[O:7].CO.Cl>O1CCCC1>[CH3:1][O:2][CH2:3][CH2:4][NH:5][S:6]([C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[CH2:12][OH:13])(=[O:8])=[O:7]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 16768026509094-14-8

生成物 1

HCID 65751811HCID 65751811、化合物収率 79.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 4.0 g of 3-[(2-methoxyethyl)aminosulfonyl]benzoic acid in 200 ml of tetrahydrofuran was added dropwise a solution of 1.07 M borane-tetrahydrofuran complex in 43.5 ml of tetrahydrofuran under ice-cooling, and this was stirred for 30 minutes, and stirred at room temperature overnight. After 40 ml of methanol was added dropwise under ice-cooling, 100 ml of 2 N hydrochloric acid was added dropwise. After warmed to room temperature, the solvent was distilled off under reduced pressure, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 3.0 g of oily 3-[(2-methoxyethyl)aminosulfonyl]benzyl alcohol.

後処理

  1. temperaturecooling
  2. stirringstirred at room temperature overnight
  3. temperaturecooling
  4. distillationthe solvent was distilled off under reduced pressure
  5. extractionfollowed by extraction with ethyl acetate
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-dc2d83c6eeed407ead967657581dc4f6
出典データセット
uspto-grants-2011_08
特許番号
US07989478B2

反応ノート

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