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Sodium Hydroxide → HCID 23077370、化合物

HRID 1373503
ノート
印刷プレビュー

反応式

HRID 1373503 の反応式
[CH2:1]([O:8][C:9]([NH:11][CH:12]([CH3:19])[CH2:13][S:14]([O:16]CC)=[O:15])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>C(O)C>[CH2:1]([O:8][C:9]([NH:11][CH:12]([CH3:19])[CH2:13][S:14]([OH:16])=[O:15])=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 23077363HCID 23077363、化合物

生成物 1

HCID 23077370HCID 23077370、化合物収率 91%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In ethanol (7 ml) was dissolved 2.2 g (7.4 mmol) of ethyl 2-(benzyloxycarbonylamino)propane-1-sulfinate, and 3.2 g (8 mmol) of 10% aqueous sodium hydroxide solution was slowly dropped thereinto under ice-cooling. The reaction was carried out at room temperature for 1 hour, after which the ethanol was distilled off and water was added to the residue, followed by two runs of extraction with methyl t-butyl ether. The aqueous layer was acidified with concentrated hydrochloric acid, followed by three runs of extraction with ethyl acetate. The extract solution was washed with saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was distilled off and the crude crystals thus obtained were washed twice with a solvent (hexane:ethyl acetate=4:1) to obtain 1.73 g (yield 91%) of 2-(benzyloxycarbonylamino)propane-1-sulfinic acid.

後処理

  1. additionwas slowly dropped
  2. temperatureunder ice-cooling
  3. distillationafter which the ethanol was distilled off
  4. additionwater was added to the residue
  5. extractionfollowed by two runs of extraction with methyl t-butyl ether
  6. extractionfollowed by three runs of extraction with ethyl acetate
  7. washThe extract solution was washed with saturated aqueous sodium chloride solution
  8. dry with materialdried over anhydrous sodium sulfate
  9. distillationThe solvent was distilled off
  10. customthe crude crystals thus obtained
  11. washwere washed twice with a solvent (hexane:ethyl acetate=4:1)

出典と根拠

ORDレコード
ord-34e034dd115a4597ac737d53b49c5b9c
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07161032B2

反応ノート

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