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Lithium Hydroxide → HCID 86690944、化合物

HRID 714737
ノート
印刷プレビュー

反応式

HRID 714737 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([CH2:13][CH:14]([OH:19])[C:15]([F:18])([F:17])[F:16])[C:11](=[O:20])[N:10]([CH2:21][C:22]3[CH:23]=[C:24]([C:32]4[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=4[C:38]([F:41])([F:40])[F:39])[CH:25]=[CH:26][C:27]=3[C:28]([O:30]C)=[O:29])[N:9]=2)=[CH:4][CH:3]=1.[OH-].[Li+]>C1COCC1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([CH2:13][CH:14]([OH:19])[C:15]([F:16])([F:17])[F:18])[C:11](=[O:20])[N:10]([CH2:21][C:22]3[CH:23]=[C:24]([C:32]4[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=4[C:38]([F:41])([F:39])[F:40])[CH:25]=[CH:26][C:27]=3[C:28]([OH:30])=[O:29])[N:9]=2)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 86690942HCID 86690942、化合物

生成物 1

HCID 86690944HCID 86690944、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

195 mg (0.36 mmol) of the compound from Example 130 were dissolved in 3 ml of THF, and 0.4 ml a 1 N aqueous lithium hydroxide solution were added. The mixture was stirred at RT for 20 h. For work-up, the solvent was removed under reduced pressure, the residue was taken up in about 5 ml of water and 0.07 ml of 6 N hydrochloric acid was added. The mixture was stirred for 15 min, and the precipitated solid was then filtered off with suction and dried under high vacuum. This gave 146 mg (73% of theory) of the target compound.

後処理

  1. customFor work-up, the solvent was removed under reduced pressure
  2. addition0.07 ml of 6 N hydrochloric acid was added
  3. stirringThe mixture was stirred for 15 min
  4. filtrationthe precipitated solid was then filtered off with suction
  5. customdried under high vacuum

出典と根拠

ORDレコード
ord-ec0966861535410a9f5027507c3631a5
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09187466B2

反応ノート

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