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Water → HCID 67361977、化合物

HRID 1183173
ノート
印刷プレビュー

反応式

HRID 1183173 の反応式
Cl.[NH2:2][C@H:3]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH3:16])[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].C(N(CC)CC)C.O.[F:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[N:32]1[C:36]([O:37][CH3:38])=[CH:35][C:34]([C:39](Cl)=[O:40])=[N:33]1>CC1CCCO1>[F:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[N:32]1[C:36]([O:37][CH3:38])=[CH:35][C:34]([C:39]([NH:2][C@H:3]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[CH3:16])[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])=[O:40])=[N:33]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 962WaterHCID 8471Triethylamine2 回HCID 67362509HCID 67362509、化合物HCID 86676960HCID 86676960、化合物2 回

生成物 1

HCID 67361977HCID 67361977、化合物

試薬・触媒・溶媒 1

HCID 73012-Methyltetrahydrofuran溶媒

実験手順

A solution of ethyl (S)-3-amino-3-(2-methyl-phenyl)-propionate hydrochloride (42.4 g, 174 mmol) in 2-methyltetrahydrofuran (200 ml) was added to the suspension of 1-(2-fluoro-phenyl)-5-methoxy-1H-pyrazole-3-carbonyl chloride in ca. 200 ml of 2-methyltetrahydrofuran obtained in step 1. Triethylamine (33.5 g, 331 mmol) was added dropwise under ice cooling. After the complete addition of the triethylamine the conversion was complete and water was added. The phases were separated and the organic phase was washed with water and evaporated. The residue was dissolved in 2-methyltetrahydrofuran (500 ml) and washed with 1 M hydrochloric acid. The organic phase was dried and the solvent was removed under reduced pressure to give 70.4 g (99% over two step) of the title compound as a light brown oil.

後処理

  1. customThe phases were separated
  2. washthe organic phase was washed with water
  3. customevaporated
  4. dissolutionThe residue was dissolved in 2-methyltetrahydrofuran (500 ml)
  5. washwashed with 1 M hydrochloric acid
  6. customThe organic phase was dried
  7. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-0c93dd7e9f494f8ab9deb90b872aa7f0
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08664257B2

反応ノート

読み込み中…

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