Hydrogen Bromide → L-alanyl-L-proline cyclohexylamide hydrobromide

HRID 1448737ノート

反応式

HRID 1448737 の反応式
[CH:1]1([NH:7][C:8](=[O:29])[C@@H:9]2[CH2:13][CH2:12][CH2:11][N:10]2[C:14](=[O:28])[C@H:15]([CH3:27])[NH:16]C(OCC2C=CC=CC=2)=O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.CCOCC.[BrH:35]>C(O)(=O)C>[BrH:35].[CH:1]1([NH:7][C:8](=[O:29])[C@@H:9]2[CH2:13][CH2:12][CH2:11][N:10]2[C:14](=[O:28])[C@H:15]([CH3:27])[NH2:16])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

参加物

5

反応物 3

HCID 260Hydrogen BromideHCID 3283Diethyl EtherHCID 53880215HCID 53880215、化合物

生成物 1

HCID 70586840L-alanyl-L-proline cyclohexylamide hydrobromide収率 100%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

2 g (0.005 mol) of N-benzyloxycarbonyl-L-alanyl-L-proline cyclohexylamide were dissolved in 10 ml of 4-N hydrogen bromide in acetic acid and the mixture was stirred at room temperature for 1 hour. 100 ml of dry ether were then added. An oil precipitated and was allowed to settle. The solution was decanted off, the oil washed with 100 ml of ether, dissolved in the minimum volume of methanol and an excess of ethyl acetate added. Crystallisation soon took place and there were obtained 1.75 g (100%) of L-alanyl-L-proline cyclohexylamide hydrobromide of melting point 233°-236° C.

後処理

  1. customAn oil precipitated
  2. customThe solution was decanted off
  3. washthe oil washed with 100 ml of ether
  4. dissolutiondissolved in the minimum volume of methanol
  5. additionan excess of ethyl acetate added
  6. customCrystallisation soon took place

出典と根拠

ORDレコード
ord-9077db9f20ed48fe81c39a06633bca84
出典データセット
uspto-grants-1980_02
特許番号
US04187216

反応ノート

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