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Tetrahydrofuran → 5-Bromo-N-(pyrimidin-4-YL)-N-((2-(trimethylsilyl)ethoxy)methyl)naphthalene-2-sulfonamide

HRID 1473364
ノート
印刷プレビュー

反応式

HRID 1473364 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([NH2:7])=[N:3][CH:2]=1.[CH3:8][Si:9]([CH2:12][CH2:13][O:14][CH2:15]Cl)([CH3:11])[CH3:10].[Br:17][C:18]1[CH:27]=[CH:26][CH:25]=[C:24]2[C:19]=1[CH:20]=[CH:21][C:22]([S:28](OC1C(F)=C(F)C(F)=C(F)C=1F)(=[O:30])=[O:29])=[CH:23]2.CC(C)([O-])C.[Li+].C1COCC1>CN(C=O)C>[Br:17][C:18]1[CH:27]=[CH:26][CH:25]=[C:24]2[C:19]=1[CH:20]=[CH:21][C:22]([S:28]([N:7]([C:4]1[CH:5]=[CH:6][N:1]=[CH:2][N:3]=1)[CH2:15][O:14][CH2:13][CH2:12][Si:9]([CH3:11])([CH3:10])[CH3:8])(=[O:29])=[O:30])=[CH:23]2
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 5

HCID 8028TetrahydrofuranHCID 689584-AminopyrimidineHCID 27242712-Chloromethyl 2-(trimethylsilyl)ethyl etherHCID 236647642-Propanol, 2-methyl-, lithium salt (1:1)HCID 86687354Perfluorophenyl 5-bromonaphthalene-2-sulfonate2 回

生成物 1

HCID 86687411
5-Bromo-N-(pyrimidin-4-YL)-N-((2-(trimethylsilyl)ethoxy)methyl)naphthalene-2-sulfonamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of pyrimidin-4-amine (0.944 g, 9.93 mmol) in 10 mL DMF was treated with SEM-Cl (1.761 ml, 9.93 mmol) and was allowed to stir at room temperature 30 minutes. Perfluorophenyl 5-bromonaphthalene-2-sulfonate (INTERMEDIATE M; 4.50 g, 9.93 mmol) was added and the reaction mixture was treated with lithium tert-butoxide 1N in THF (19.86 ml, 19.86 mmol) drop wise. After stirring for one hour, the reaction mixture was concentrated. The crude residue was diluted with DCM, washed with water, the organics dried over MgSO4 and concentrated. The material (INTERMEDIATE CCC) was carried forward crude without further purification.

後処理

  1. stirringAfter stirring for one hour
  2. concentrationthe reaction mixture was concentrated
  3. additionThe crude residue was diluted with DCM
  4. washwashed with water
  5. dry with materialthe organics dried over MgSO4
  6. concentrationconcentrated
  7. customwithout further purification

出典と根拠

ORDレコード
ord-ced9276fac1948328149ad3fe9cf87f4
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09012443B2

反応ノート

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