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N,N-Dimethylglycine → HCID 68501766、化合物

HRID 1714022
ノート
印刷プレビュー

反応式

HRID 1714022 の反応式
[CH:1]1([C:7]2[C:8]3[CH:9]=[CH:10][C:11]([C:27]([O:29][CH3:30])=[O:28])=[CH:12][C:13]=3[N:14]3[CH2:21][CH2:20][NH:19][CH2:18][C:17]4[CH:22]=[C:23]([F:26])[CH:24]=[CH:25][C:16]=4[C:15]=23)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.CCN(C(C)C)C(C)C.[CH3:40][N:41]([CH3:46])[CH2:42][C:43](O)=[O:44].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>C(Cl)Cl.Cl>[CH:1]1([C:7]2[C:8]3[CH:9]=[CH:10][C:11]([C:27]([O:29][CH3:30])=[O:28])=[CH:12][C:13]=3[N:14]3[CH2:21][CH2:20][N:19]([C:43](=[O:44])[CH2:42][N:41]([CH3:46])[CH3:40])[CH2:18][C:17]4[CH:22]=[C:23]([F:26])[CH:24]=[CH:25][C:16]=4[C:15]=23)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 673N,N-DimethylglycineHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 68507183HCID 68507183、化合物

生成物 1

HCID 68501766HCID 68501766、化合物

試薬・触媒・溶媒 2

HCID 313
Hydrochloric Acid
溶媒
HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of methyl 14-cyclohexyl-3-fluoro-5,6,7,8-tetrahydroindolo[2,1-a][2,5]benzodiazocine-11-carboxylate (from Step 5) in DCM (0.15 M), DIPEA (4 eq.), dimethylglycine (3 eq.) and HATU (2 eq.) were added and the mixture stirred at RT overnight. The solution was diluted with DCM and HCl (1N) and the 2 phases separated. The aqueous phase was extracted with DCM (twice). The combined organic phases were then washed with a saturated aqueous solution of NaHCO3 and brine before being dried (Na2SO4), filtered and concentrated in vacuo. The crude was used in the next step without further purification; MS (ES+) m/z 492 (M+H)+.

後処理

  1. customthe 2 phases separated
  2. extractionThe aqueous phase was extracted with DCM (twice)
  3. washThe combined organic phases were then washed with a saturated aqueous solution of NaHCO3 and brine
  4. dry with materialbefore being dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe crude was used in the next step without further purification

出典と根拠

ORDレコード
ord-8f2bdac398294fe5969c1edb41002629
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07795247B2

反応ノート

読み込み中…

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