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Diisopropylethylamine → HCID 178513886、化合物

HRID 1655739
ノート
印刷プレビュー

反応式

HRID 1655739 の反応式
N[C@@H:2]([CH2:23][C:24]1[N:25]=[CH:26][NH:27][CH:28]=1)[C:3]([NH:5][C@@H](CC1CCCCC1)[C@@H](O)C[C@@H](C(C)C)C=C)=[O:4].CCN(C(C)C)C(C)C.O1CCN(NC(N[C@H](C(O)=O)CC2C=CC=CC=2)=O)CC1.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1>C(#N)C>[NH:27]1[CH:28]=[C:24]([CH2:23][CH2:2][C:3]([NH2:5])=[O:4])[N:25]=[CH:26]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 54167396N-(morpholinocarbamoyl)-3-phenyl-L-alanineHCID 178456019HCID 178456019、化合物

生成物 1

HCID 178513886HCID 178513886、化合物

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒
2 回

実験手順

100 mg (0.52 mmol) of (S)-α-amino- N-[(1S,2S,4S)-1-(cyclohexylmethyl)-2-hydroxy-4-isopropyl-5-hexenyl]imidazole-4-propionamide and 0.052 ml of Hunig base in 2 ml of acetonitrile were treated at room temperature with 99 mg of N-(morpholinocarbamoyl)-3-phenyl-L-alanine and 113 mg of BOP in 2 ml of acetonitrile and stirred at room temperature for 12 hours. Thereafter, the reaction solution was poured onto 1N hydrochloric acid/ice, extracted with ethyl acetate, the organic extracts were dried over sodium sulfate and the solvent was removed under reduced pressure. The residue was chromatoqraphed on silica gel with a 10:1 mixture of methylene chloride and methanol, to obtain 130 mg (67%) of (S)-N-[(1S,2S,4S)-1-(cyclohexyl-methyl)-2-hydroxy-4-isopropyl-5 hexenyl]-α-2-[N-(morpholinocarbamoyl)-3-phenyl-L-alanyl]amino]imidazole-4-propionamide as an amorphous solid. MS: 651 (M+H)+.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialthe organic extracts were dried over sodium sulfate
  3. customthe solvent was removed under reduced pressure
  4. additionThe residue was chromatoqraphed on silica gel with a 10:1 mixture of methylene chloride and methanol

出典と根拠

ORDレコード
ord-ec360e3ff1b444649f98fd379a247f5d
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05250517

反応ノート

読み込み中…

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