Sodium Hydroxide → HCID 22247174、化合物

HRID 2121862ノート

反応式

HRID 2121862 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([CH:22]=[O:23])=[C:13]([N:15]([CH2:18][CH:19]([OH:21])[CH3:20])C=O)[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>C1COCC1>[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([CH:22]=[O:23])=[C:13]([NH:15][CH2:18][CH:19]([OH:21])[CH3:20])[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 22247178N-(5-Benzyloxy-2-formylphenyl)-N-(2-hydroxypropyl)-formamide

生成物 1

HCID 22247174HCID 22247174、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

An ice-cooled solution of the product from Step B (298 g, 0.95 mol) in THF (3 L) was treated with 1 M aqueous sodium hydroxide (1.95 L, 1.9 mol) keeping the temperature below 8° C. After the starting material was consumed, the mixture was diluted with brine and extracted twice with ethyl ether. The organic solution was washed with water until neutral and then with brine, dried over sodium sulfate, treated with charcoal and passed through silica (1 kg) with ether and with 1:1 ethyl acetate-hexane to yield, after concentration in vacuo, a yellow solid (207 g, 76%).

後処理

  1. customthe temperature below 8° C
  2. customAfter the starting material was consumed
  3. additionthe mixture was diluted with brine
  4. extractionextracted twice with ethyl ether
  5. washThe organic solution was washed with water until neutral and then with brine
  6. dry with materialdried over sodium sulfate
  7. additiontreated with charcoal
  8. customto yield
  9. concentrationafter concentration in vacuo

出典と根拠

ORDレコード
ord-054df37d290844e1b540be7e8c8bdcc9
出典データセット
uspto-grants-2004_02
特許番号
US06696476B2

反応ノート

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