Phenyl chloroformate → HCID 59379937、化合物

HRID 2353729ノート

反応式

HRID 2353729 の反応式
Cl[C:2]([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:3].[F:11][C:12]1[CH:17]=[CH:16][C:15]([S:18]([C:21]([C:24]2[CH:29]=[C:28]([N:30]3[CH2:35][CH2:34][O:33][CH2:32][C@@H:31]3[CH3:36])[N:27]=[C:26]([C:37]3[CH:43]=[CH:42][C:40]([NH2:41])=[CH:39][CH:38]=3)[N:25]=2)([CH3:23])[CH3:22])(=[O:20])=[O:19])=[CH:14][CH:13]=1.C(=O)(O)[O-].[Na+]>O1CCOCC1>[F:11][C:12]1[CH:17]=[CH:16][C:15]([S:18]([C:21]([C:24]2[CH:29]=[C:28]([N:30]3[CH2:35][CH2:34][O:33][CH2:32][C@@H:31]3[CH3:36])[N:27]=[C:26]([C:37]3[CH:38]=[CH:39][C:40]([NH:41][C:2](=[O:3])[O:4][C:5]4[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=4)=[CH:42][CH:43]=3)[N:25]=2)([CH3:22])[CH3:23])(=[O:19])=[O:20])=[CH:14][CH:13]=1

参加物

5

反応物 3

HCID 15891Phenyl chloroformateHCID 516892Sodium BicarbonateHCID 59379869HCID 59379869、化合物

生成物 1

HCID 59379937HCID 59379937、化合物収率 99.9%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Phenyl chloroformate (0.482 mL, 3.83 mmol) was added dropwise to 4-[4-[2-(4-fluorophenyl)sulfonylpropan-2-yl]-6-[(3S)-3-methylmorpholin-4-yl]pyrimidin-2-yl]aniline (1.8 g, 3.83 mmol) and sodium bicarbonate (0.482 g, 5.74 mmol) in dioxane (20 mL) under nitrogen. The resulting suspension was stirred at RT for 2 hours. The reaction mixture was evaporated to dryness and redissolved in DCM (50 mL) and washed with water (50 mL). The organic layer was dried (MgSO4), filtered and evaporated to give crude product which was triturated with diethyl ether to give the desired material as a white solid (2.26 g).

後処理

  1. customThe reaction mixture was evaporated to dryness
  2. dissolutionredissolved in DCM (50 mL)
  3. washwashed with water (50 mL)
  4. dry with materialThe organic layer was dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated
  7. customto give crude product which
  8. customwas triturated with diethyl ether

出典と根拠

ORDレコード
ord-2ece19b68d18457ba377f6c07b8d0764
出典データセット
uspto-grants-2010_07
特許番号
US07750003B2

反応ノート

読み込み中…