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Methanol → (R)-tert-butyl 3-amino-3-(3-fluoro-4-(trifluoromethyl)phenyl)propylcarbamate

HRID 2279535
ノート
印刷プレビュー

反応式

HRID 2279535 の反応式
O=C1C2C(=CC=CC=2)C(=O)[N:3]1[C@@H:12]([C:23]1[CH:28]=[CH:27][C:26]([C:29]([F:32])([F:31])[F:30])=[C:25]([F:33])[CH:24]=1)[CH2:13][CH2:14][NH:15][C:16](=[O:22])[O:17][C:18]([CH3:21])([CH3:20])[CH3:19].CO.C1COCC1.O.NN>O>[NH2:3][C@@H:12]([C:23]1[CH:28]=[CH:27][C:26]([C:29]([F:30])([F:31])[F:32])=[C:25]([F:33])[CH:24]=1)[CH2:13][CH2:14][NH:15][C:16](=[O:22])[O:17][C:18]([CH3:21])([CH3:19])[CH3:20]
参加物反応条件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 887MethanolHCID 8028TetrahydrofuranHCID 24654Hydrazine hydrate (1:1)HCID 68294223(R)-tert-butyl 3-(1,3-dioxoisoindolin-2-yl)-3-(3-fluoro-4-(trifluoromethyl)phenyl)propylcarbamate

生成物 1

HCID 86705529(R)-tert-butyl 3-amino-3-(3-fluoro-4-(trifluoromethyl)phenyl)propylcarbamate収率 59.5%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

反応条件

温度
50 °C

実験手順

To a solution of 288 (0.350 g, 0.750 mmol) and MeOH:THF (6 mL, 1:1) was added hydrazine monohydrate (0.188 mL, 3.75 mmol) and the reaction was heated to 50° C. for 4 d. The reaction was then poured into water, and extracted with DCM. The combined organic extracts were dried (MgSO4), filtered, and concentrated in vacuo. The crude product was purified by SiO2 chromatography eluting with DCM/MeOH (500:20) to afford 0.150 g (59.4%) of (R)-tert-butyl 3-amino-3-(3-fluoro-4-(trifluoromethyl)phenyl)propylcarbamate (290).

後処理

  1. extractionextracted with DCM
  2. dry with materialThe combined organic extracts were dried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by SiO2 chromatography
  6. washeluting with DCM/MeOH (500:20)

出典と根拠

ORDレコード
ord-ce09d9c392504c45bb5e23f0e05a1984
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133187B2

反応ノート

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