(+)-4,5-dihydro-1-[[[(2,2-dimethyl-1-oxopropoxy)methoxy](4-phenylbutyl)phosphinyl]acetyl]-3-phenyl-1H-pyrazole-5-carboxylic acid, phenylmethyl ester → (+)-4,5-dihydro-1-[[[(2,2-dimethyl-1-oxopropoxy)methoxy] (4-phenylbutyl)phosphinyl]acetyl]-3-phenyl-1H-pyrazole-5-carboxylic acid

HRID 1757942ノート

反応式

HRID 1757942 の反応式
[CH3:1][C:2]([CH3:45])([CH3:44])[C:3](=[O:43])[O:4][CH2:5][O:6][P:7]([CH2:19][C:20]([N:22]1[CH:26]([C:27]([O:29]CC2C=CC=CC=2)=[O:28])[CH2:25][C:24]([C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=2)=[N:23]1)=[O:21])([CH2:9][CH2:10][CH2:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:8].[H][H]>[Pd].CO>[CH3:1][C:2]([CH3:45])([CH3:44])[C:3](=[O:43])[O:4][CH2:5][O:6][P:7]([CH2:19][C:20]([N:22]1[CH:26]([C:27]([OH:29])=[O:28])[CH2:25][C:24]([C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=2)=[N:23]1)=[O:21])([CH2:9][CH2:10][CH2:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:8]

参加物

5

反応物 2

HCID 86738775(+)-4,5-dihydro-1-[[[(2,2-dimethyl-1-oxopropoxy)methoxy](4-phenylbutyl)phosphinyl]acetyl]-3-phenyl-1H-pyrazole-5-carboxylic acid, phenylmethyl esterHCID 178418361HCID 178418361、化合物

生成物 1

HCID 20510338(+)-4,5-dihydro-1-[[[(2,2-dimethyl-1-oxopropoxy)methoxy] (4-phenylbutyl)phosphinyl]acetyl]-3-phenyl-1H-pyrazole-5-carboxylic acid

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

The diester product from part (d) (2.0 g.) is dissolved in 50 ml. of methanol containing 0.5 g. of 5% palladium on carbon catalyst and hydrogenated at 50 psi on a Parr apparatus until cessation of hydrogen uptake (2-4 hours). The catalyst is filtered off and the filtrate is concentrated in vacuo. The residue is triturated with acetonitrile or purified by flash chromatography to give (+)-4,5-dihydro-1-[[[(2,2-dimethyl-1-oxopropoxy)methoxy] (4-phenylbutyl)phosphinyl]acetyl]-3-phenyl-1H-pyrazole-5-carboxylic acid.

後処理

  1. filtrationThe catalyst is filtered off
  2. concentrationthe filtrate is concentrated in vacuo
  3. customThe residue is triturated with acetonitrile
  4. custompurified by flash chromatography

出典と根拠

ORDレコード
ord-507bfdfd7d2d48c5b1c770bb4ddb094a
出典データセット
uspto-grants-1983_02
特許番号
US04371526

反応ノート

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