Hydrazine hydrate (1:1) → (S)-3-[[(6-aminohexyl)ethoxyphosphinyl]amino]-2-oxo-1-piperidineacetic acid, ethyl ester

HRID 1285473ノート

反応式

HRID 1285473 の反応式
[CH2:1]([O:3][P:4]([NH:23][C@H:24]1[CH2:29][CH2:28][CH2:27][N:26]([CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])[C:25]1=[O:36])([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][N:12]1C(=O)C2=CC=CC=C2C1=O)=[O:5])[CH3:2].O.NN>O1CCOCC1.C1(C)C=CC=CC=1>[NH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][P:4]([NH:23][C@H:24]1[CH2:29][CH2:28][CH2:27][N:26]([CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])[C:25]1=[O:36])([O:3][CH2:1][CH3:2])=[O:5]

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 86740217(S)-3-[[ethoxy(6-phthalimidohexyl)phosphinyl]amino]-2-oxo-1-piperidineacetic acid, ethyl ester

生成物 1

HCID 86740218(S)-3-[[(6-aminohexyl)ethoxyphosphinyl]amino]-2-oxo-1-piperidineacetic acid, ethyl ester

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of (S)-3-[[ethoxy(6-phthalimidohexyl)phosphinyl]amino]-2-oxo-1-piperidineacetic acid, ethyl ester in dioxane is treated with hydrazine hydrate and stirred at room temperature under argon. After the reaction is completed, the mixture is diluted with toluene and the solvents decanted. The residue is triturated with methylene chloride and filtered. The combined filtrate is evaporated to dryness to give (S)-3-[[(6-aminohexyl)ethoxyphosphinyl]amino]-2-oxo-1-piperidineacetic acid, ethyl ester.

後処理

  1. customthe solvents decanted
  2. customThe residue is triturated with methylene chloride
  3. filtrationfiltered
  4. customThe combined filtrate is evaporated to dryness

出典と根拠

ORDレコード
ord-6e11aecd3f0a490cb7bc9efb294199dd
出典データセット
uspto-grants-1986_01
特許番号
US04567167

反応ノート

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