Phosphoric Acid → HCID 58972470、化合物

HRID 30993ノート

反応式

HRID 30993 の反応式
[CH3:1][O:2][C:3](=[O:29])[CH2:4][N:5]1[C:11](=[O:12])[C@@H:10]([NH:13]C(OC(C)(C)C)=O)[C:9]2[CH:21]=[CH:22][CH:23]=[CH:24][C:8]=2[C:7]2[CH:25]=[CH:26][CH:27]=[CH:28][C:6]1=2.P(=O)(O)(O)O.[OH-].[Na+]>ClCCl>[CH3:1][O:2][C:3](=[O:29])[CH2:4][N:5]1[C:11](=[O:12])[C@@H:10]([NH2:13])[C:9]2[CH:21]=[CH:22][CH:23]=[CH:24][C:8]=2[C:7]2[CH:25]=[CH:26][CH:27]=[CH:28][C:6]1=2

参加物

5

反応物 3

HCID 1004Phosphoric AcidHCID 14798Sodium HydroxideHCID 58972533((S)-7-tert-Butoxycarbonylamino-6-oxo-6,7-dihydro-dibenzo[b,d]azepin-5-yl)-acetic acid methyl ester

生成物 1

HCID 58972470HCID 58972470、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

((S)-7-tert-Butoxycarbonylamino-6-oxo-6,7-dihydro-dibenzo[b,d]azepin-5-yl)-acetic acid methyl ester (60 mg, 0.15 mmol) were dissolved in dichloromethane (3 ml), treated with 0.15 ml (2.3 mmol) orthophosphoric acid and stirred for 18 .h The reaction mixture is adjusted to pH 7.5 with 2N aqueous sodium hydroxide, diluted with dichloromethane (5 ml) and the phases separated. After extraction of the organic phases with water (5 ml) and saturated aqueous sodium chloride (5 ml), the solution is dried with magnesium sulfate and evaporated to dryness. White solid (60%); MS: m/e=297(M+H+), which was used without further purification.

後処理

  1. customthe phases separated
  2. extractionAfter extraction of the organic phases with water (5 ml) and saturated aqueous sodium chloride (5 ml)
  3. dry with materialthe solution is dried with magnesium sulfate
  4. customevaporated to dryness
  5. customMS: m/e=297(M+H+), which was used without further purification

出典と根拠

ORDレコード
ord-50155863f6ec4ac090cace69e4b37baf
出典データセット
uspto-grants-2008_09
特許番号
US07425551B2

反応ノート

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