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Diisopropylethylamine → HCID 71060508、化合物

HRID 1036673
ノート
印刷プレビュー

反応式

HRID 1036673 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[C:12]3([CH2:17][CH2:16][CH2:15][NH:14][CH2:13]3)[C:11](=[O:18])[N:10]([CH:19]([CH3:21])[CH3:20])[CH2:9]2)=[CH:4][CH:3]=1.[C:22]([O:26][C:27]([NH:29][C:30]([CH3:50])([CH3:49])[C:31]([NH:33][C@H:34]([CH2:38][C:39]1[C:47]2[C:42](=[CH:43][CH:44]=[CH:45][CH:46]=2)[N:41]([CH3:48])[CH:40]=1)[C:35](O)=[O:36])=[O:32])=[O:28])([CH3:25])([CH3:24])[CH3:23].CCN(C(C)C)C(C)C.C(P1(=O)OP(CCC)(=O)OP(CCC)(=O)O1)CC>C(#N)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[C:12]3([CH2:17][CH2:16][CH2:15][N:14]([C:35](=[O:36])[C@H:34]([NH:33][C:31](=[O:32])[C:30]([NH:29][C:27](=[O:28])[O:26][C:22]([CH3:24])([CH3:23])[CH3:25])([CH3:50])[CH3:49])[CH2:38][C:39]4[C:47]5[C:42](=[CH:43][CH:44]=[CH:45][CH:46]=5)[N:41]([CH3:48])[CH:40]=4)[CH2:13]3)[C:11](=[O:18])[N:10]([CH:19]([CH3:21])[CH3:20])[CH2:9]2)=[CH:6][CH:7]=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 111923Propylphosphonic anhydrideHCID 710602794-(4-Fluorophenyl)-2-(1-methylethyl)-2,7-diazaspiro[4.5]decan-1-oneHCID 71060485HCID 71060485、化合物2 回

生成物 1

HCID 71060508HCID 71060508、化合物

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

実験手順

A mixture comprising 4-(4-fluorophenyl)-2-isopropyl-2,7-diazaspiro[4.5]decan-1-one (ASW MedChem) (243 mg, 0.744 mmol), (R)-2-(2-(tert-butoxycarbonylamino)-2-methylpropanamido)-3-(1-methyl-1H-indol-3-yl)propanoic acid (Intermediate 3D) (300 mg, 0.744 mmol) and DIPEA (0.519 ml, 2.97 mmol) in acetonitrile (3 ml) was treated with ®T3P (50% in DMF, 0.868 ml, 1.487 mmol) and stirred at RT for 19 hours. The reaction mixture was concentrated in vacuo, dissolved in EtOAc and washed with water. The organic portion was dried (MgSO4) and concentrated in vacuo. Purification of the crude product by chromatography on silica eluting with 2% MeOH in DCM afforded the title compound;

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. dissolutiondissolved in EtOAc
  3. washwashed with water
  4. dry with materialThe organic portion was dried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customPurification of the crude product by chromatography on silica eluting with 2% MeOH in DCM

出典と根拠

ORDレコード
ord-d43da3bbd4e944ed8678992567d416ca
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08546416B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート