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Chloride → HCID 11670829、化合物

HRID 33981
ノート
印刷プレビュー

反応式

HRID 33981 の反応式
CS(C)=O.[Cl-].[OH:6][CH:7]([CH2:36][CH2:37][C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)[CH2:8][N:9]1[C:14]2=[N:15][C:16]([C:30]3[CH:35]=[CH:34][N:33]=[CH:32][CH:31]=3)=[C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:29])([F:28])[F:27])[CH:21]=3)[C:18](=[O:19])[N:13]2[CH2:12][CH2:11][CH2:10]1.CCN(CC)CC>C(Cl)Cl>[O:6]=[C:7]([CH2:36][CH2:37][C:38]1[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=1)[CH2:8][N:9]1[C:14]2=[N:15][C:16]([C:30]3[CH:35]=[CH:34][N:33]=[CH:32][CH:31]=3)=[C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:29])([F:28])[F:27])[CH:21]=3)[C:18](=[O:19])[N:13]2[CH2:12][CH2:11][CH2:10]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 312ChlorideHCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 597965069-(2-Hydroxy-4-phenyl-butyl)-2-pyridin-4-yl-3-(3-trifluoromethyl-phenyl)-6,7,8,9-tetrahydro-pyrimido[1,2-a]pyrimidin-4-one

生成物 1

HCID 11670829HCID 11670829、化合物収率 66.4%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
3 回

実験手順

A solution of DMSO (0.25 mL, 3.5 mmol) in CH2Cl2 (10 mL) at −78 C was treated with a solution of oxallyl chloride (2N in CH2Cl2, 0.8 mL, 1.6 mmol) dropwise. After stirring for 15 min, a solution of 9-(2-hydroxy-4-phenyl-butyl)-2-pyridin-4-yl-3-(3-trifluoromethyl-phenyl)-6,7,8,9-tetrahydro-pyrimido[1,2-a]pyrimidin-4-one (227 mg, 0.43 mmol) in CH2Cl2 (15 mL) was added. The mixture was stirred at −60 C for 15 min before a solution of Et3N (0.5 mL, 3.6 mmol) in CH2Cl2 (3 mL) was added. The reaction mixture was allowed to warm to room temperature overnight and was washed with NaHCO3 (aq). The organic layer was dired (Na2SO4), and concentrated. The residue was eluted on silica gel with 0-5% (2N NH3-MeOH in CH2Cl2) to afford the product as a light yellow solid (148 mg, 63%). M+1 519.

後処理

  1. additionwas added
  2. washwas washed with NaHCO3 (aq)
  3. concentrationconcentrated
  4. washThe residue was eluted on silica gel with 0-5% (2N NH3-MeOH in CH2Cl2)

出典と根拠

ORDレコード
ord-0e3c6dd3a80d4d95964ac69d7cb58630
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07429594B2

反応ノート

読み込み中…

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