Trityl chloride → amino-1-cyclohexyl-3(S)-hydroxy-6-methylheptane

HRID 1649924ノート

反応式

HRID 1649924 の反応式
CN[C@H](C(N[C@H:13]([C@@H:21]([OH:27])[CH2:22][CH2:23][CH:24]([CH3:26])[CH3:25])[CH2:14][CH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1)=O)CC1N=CNC=1.C([N:30](CC)CC)C.C(Cl)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>C(Cl)Cl>[NH2:30][CH:14]([CH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1)[CH2:13][C@@H:21]([OH:27])[CH2:22][CH2:23][CH:24]([CH3:26])[CH3:25]

参加物

5

反応物 3

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 178484877HCID 178484877、化合物

生成物 1

HCID 57008919amino-1-cyclohexyl-3(S)-hydroxy-6-methylheptane収率 270.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2(S)-(Nα -methyl-L-histidyl)amino-1-cyclohexyl-3(S)-hydroxy-6-methylheptane (900 mg) and triethylamine (494 mg) in methylene chloride (20 ml) was added trityl chloride (696 mg) at 0° C. The mixture was stirred at the same temperature for 1 hour. After evaporation of the solvent, the residue was dissolved in ethyl acetate (30 ml) and the solution was washed with 1M sodium bicarbonate solution and water successively, and dried over magnesium.sulfate. Evaporation of the solvent gave 2(S)-(Nα -methyl-Nim -trityl-L-histidyl)amino-1-cyclohexyl-3(S)-hydroxy-6-methylheptane (1.46 g) as an amorphous powder.

後処理

  1. customAfter evaporation of the solvent
  2. dissolutionthe residue was dissolved in ethyl acetate (30 ml)
  3. washthe solution was washed with 1M sodium bicarbonate solution and water successively
  4. dry with materialdried over magnesium
  5. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-6cef93508e844c3099ee7e1e90a3b07e
出典データセット
uspto-grants-1990_05
特許番号
US04921855

反応ノート

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