Triethylamine → HCID 178448490、化合物

HRID 254618

反応式

HRID 254618 の反応式
I.[CH2:2]([N:6]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[S:8][C:7]1=[NH:15])[CH2:3][CH2:4][CH3:5].C(N(CC)CC)C.[Cl:23][C:24]1[CH:25]=[CH:26][C:27]([O:33][CH3:34])=[C:28]([CH:32]=1)[C:29](Cl)=[O:30]>C(Cl)Cl>[CH2:2]([N:6]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[S:8]/[C:7]/1=[N:15]\[C:29](=[O:30])[C:28]1[CH:32]=[C:24]([Cl:23])[CH:25]=[CH:26][C:27]=1[O:33][CH3:34])[CH2:3][CH2:4][CH3:5]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 123841765-Chloro-2-methoxybenzoyl chlorideHCID 668521773-butyl-5-tert-butyl-1,3-thiazol-2(3H)-imine hydroiodide

生成物 1

HCID 178448490HCID 178448490、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of Example 6A (1.4 g, ˜4 mmol) and triethylamine (1.4 mL, 10 mmol) in CH2Cl2 (35 mL) at 0° C. was added 5-chloro-2-methoxy-benzoyl chloride (820 mg, 4 mmol), the mixture was allowed to warm to room temperature was stirred for 14 hours. The mixture was washed sequentially with water, brine, dried with anhydrous MgSO4, filtered and concentrated under reduced pressure. The residue was purified by chromatography (6:2:2 Hexane-EtOAc-CH2Cl2) to provide the title compound. 1H NMR (300 MHz, DMSO-d6) δ: 0.94 (t, J=7 Hz, 3H), 1.30 (m+s, 11H), 1.75 (m, 2H), 3.77 (s, 3H), 4.14 (t, J=7 Hz, 2H), 7.10 (d, J=9 Hz, 1H), 7.31 (s, 1H), 7.43 (d-d, J=9 Hz, 3 Hz, 1H), 7.65 (d, J=3 Hz, 1H); MS (ESI+) m/z 381 (M+H)+.

後処理

  1. washThe mixture was washed sequentially with water, brine
  2. dry with materialdried with anhydrous MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by chromatography (6:2:2 Hexane-EtOAc-CH2Cl2)

出典と根拠

ORDレコード
ord-ee0b6dfc72374d449795fd3ab4b79bfa
出典データセット
uspto-grants-2011_01
特許番号
US07875640B2

関連ノート

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