Methanol → 12-Aminododecanoic Acid

HRID 260938

反応式

HRID 260938 の反応式
[O:1]=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13](=[N:15]O)O.[H][H].C[OH:20]>[Pt]=O>[NH2:15][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][C:2]([OH:20])=[O:1]

参加物

5

反応物 3

HCID 887Methanol2 回HCID 178418361HCID 178418361、化合物HCID 178520596HCID 178520596、化合物

生成物 1

HCID 6966112-Aminododecanoic Acid収率 92%

試薬・触媒・溶媒 1

HCID 82844Platinum oxide (PtO)触媒

実験手順

In a paar hydrogenation bottle was placed 0.92 g (4×10-3 mol) 12-oxododecanoic acid oxime, 10 mL methanol, and then 0.005 g (2.2×10-5 mol) platinum oxide (Adam's catalyst). The bottle was fitted to a paar high-pressure system, deaerated, deaerated, then filled with hydrogen gas to maintain a pressure of about 3 atm for 1.5 hours with continuous shaking. After hydrogenation, 10 mL of methanol was added to the reaction mixture, then heated to gentle boiling to dissolve the product. The hot mixture was quickly filtered to remove suspension of black platinum, after which the filtrate on evaporation gave 0.85 g (92% yield) 12-aminododecanoic acid. Recrystallization was effected with ethanol/water mixture (1:1) to give 0.80 g (87% yield) 12-aminododecanoic acid (m.p. 184°-186° C., Lit. 185°-187° C.).

後処理

  1. customThe bottle was fitted to a paar high-pressure system
  2. temperatureto maintain a pressure of about 3 atm for 1.5 hours with continuous shaking
  3. temperatureheated to gentle boiling
  4. dissolutionto dissolve the product
  5. filtrationThe hot mixture was quickly filtered
  6. customto remove
  7. additionsuspension of black platinum
  8. customafter which the filtrate on evaporation

出典と根拠

ORDレコード
ord-e63459e9ae694a3aa7ff3b40e81946ec
出典データセット
uspto-grants-1996_06
特許番号
US05530148

関連ノート

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