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

HRID 1734568
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반응식

HRID 1734568 반응식
[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
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참가 물질

4

반응물 2

HCID 23022601,3,8-Triazaspiro(4.5)decane-2,4-dione, 8-methyl-HCID 17749109Barium hydroxide, octahydrate

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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 liltrate was neutralized with solid carbon dioxide and the precipitate was removed by filtration. The liltrate was concentrated to a small volume to give 4-amino-l-methylpiperidine-4-carboxylic acid (32.0 g., 95% yield), m.p. 275°-280° C. (dec.).

후처리

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

출처 및 근거

ORD 기록
ord-ea19af42e33d4c29990d6b309f91dfe5
출처 데이터셋
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05534520

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