Hydrochloric Acid → HCID 57780986、化合物

HRID 1011227ノート

反応式

HRID 1011227 の反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([O:23][CH3:24])[C:11]=1[N:12]1[CH2:17][CH2:16][CH:15]([C:18]([O:20]CC)=[O:19])[CH2:14][CH2:13]1)[N:8]([CH2:25][CH2:26][F:27])[CH:7]=[C:6]([C:28]([NH:30][CH2:31][C:32]1[CH:37]=[CH:36][C:35]([O:38][C:39]([F:42])([F:41])[F:40])=[CH:34][C:33]=1[CH3:43])=[O:29])[C:5]2=[O:44].[OH-].[Li+].Cl>O1CCOCC1.C(OCC)(=O)C.O>[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([O:23][CH3:24])[C:11]=1[N:12]1[CH2:13][CH2:14][CH:15]([C:18]([OH:20])=[O:19])[CH2:16][CH2:17]1)[N:8]([CH2:25][CH2:26][F:27])[CH:7]=[C:6]([C:28]([NH:30][CH2:31][C:32]1[CH:37]=[CH:36][C:35]([O:38][C:39]([F:42])([F:40])[F:41])=[CH:34][C:33]=1[CH3:43])=[O:29])[C:5]2=[O:44]

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 57781005HCID 57781005、化合物

生成物 1

HCID 57780986HCID 57780986、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

60 mg (0.096 mmol) of the compound of Example 4 are dissolved in 2.35 ml of dioxane, 480 μl (5 eq.) of a 1M solution of lithium hydroxide are added, and the mixture is stirred at RT until the reaction is complete (4 h). The reaction mixture is acidified with 1N hydrochloric acid and diluted with ethyl acetate and water. Following phase separation, the organic phase is washed once again with water and then with a saturated sodium chloride solution, dried over magnesium sulfate and freed from solvents on a rotary evaporator. The residue is dried under high vacuum. 54 mg (94% of theory) of the title compound are obtained.

後処理

  1. custom(4 h)
  2. customFollowing phase separation
  3. washthe organic phase is washed once again with water
  4. dry with materialwith a saturated sodium chloride solution, dried over magnesium sulfate
  5. customfreed from solvents on a rotary evaporator
  6. customThe residue is dried under high vacuum

出典と根拠

ORDレコード
ord-915291128ce9417094a5cafe476c59c8
出典データセット
uspto-grants-2011_07
特許番号
US07977349B2

反応ノート

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