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1,3,8-Triazaspiro(4.5)decane-2,4-dione, 8-methyl- → 4-Amino-1-methylpiperidine-4-carboxylic acid

HRID 1654490
ノート
印刷プレビュー

反応式

HRID 1654490 の反応式
[CH3:1][N:2]1[CH2:13][CH2:12][C:5]2([NH:9]C(=O)N[C:6]2=[O:11])[CH2:4][CH2:3]1.[OH2:14].O.O.O.O.O.O.O.[OH-].[Ba+2].[OH-]>O>[NH2:9][C:5]1([C:6]([OH:11])=[O:14])[CH2:4][CH2:3][N:2]([CH3:1])[CH2:13][CH2:12]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 23022601,3,8-Triazaspiro(4.5)decane-2,4-dione, 8-methyl-HCID 17749109Barium hydroxide, octahydrate

生成物 1

HCID 2729544-Amino-1-methylpiperidine-4-carboxylic acid収率 2,215.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1 -methylpiperidine-4-spiro-5'-hydantoin (9.75 g., 0.0533 mole) and barium hydroxide octahydrate (28.8 g., 0.00913 mole) in water (150 ml.) were heated at 160° C. in an autoclave for three hours. The contents of four such batches were combined and the precipitated barium carbonate was filtered off. The filtrate was neutralized with solid carbon dioxide and the precipitate was removed by filtration. The filtrate was concentrated to a small volume to give 4-amino-1-methylpiperidine-4-carboxylic acid (32.0 g., 95% yield), m.p. 275°-280° C. (dec.).

後処理

  1. filtrationthe precipitated barium carbonate was filtered off
  2. customthe precipitate was removed by filtration
  3. concentrationThe filtrate was concentrated to a small volume

出典と根拠

ORDレコード
ord-b6d3eafd24234920899b8ed115361724
出典データセット
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05407938

反応ノート

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