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Acetic Acid → HCID 44243038、化合物

HRID 1013090
ノート
印刷プレビュー

反応式

HRID 1013090 の反応式
OC(C(F)(F)F)=O.[NH2:8][C:9]1([C:32]([NH2:34])=[O:33])[CH2:14][CH2:13][N:12]([C:15]([C:17]2[C:18]3[CH:31]=[CH:30][CH:29]=[CH:28][C:19]=3[S:20][C:21]=2[NH:22][C:23]([NH:25][CH2:26][CH3:27])=[O:24])=[O:16])[CH2:11][CH2:10]1.C(O)(=O)C.[CH2:39]([O:41][C:42](OCC)([O:50]CC)[CH2:43][CH2:44][C:45](OCC)=O)[CH3:40]>C1(C)C=CC=CC=1.CN(C=O)C>[CH2:26]([NH:25][C:23](=[O:24])[NH:22][C:21]1[S:20][C:19]2[CH:28]=[CH:29][CH:30]=[CH:31][C:18]=2[C:17]=1[C:15]([N:12]1[CH2:11][CH2:10][C:9]2([N:8]=[C:45]([CH2:44][CH2:43][C:42]([O:41][CH2:39][CH3:40])=[O:50])[NH:34][C:32]2=[O:33])[CH2:14][CH2:13]1)=[O:16])[CH3:27]
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 3

HCID 176Acetic AcidHCID 13452377Ethyl 4,4,4-triethoxybutanoateHCID 44243036HCID 44243036、化合物

生成物 1

HCID 44243038HCID 44243038、化合物収率 65%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
85 °C

実験手順

4-Amino-1-(2-(3-ethylureido)benzo[b]thiophene-3-carbonyl)piperidine-4-carboxamide (7, 100 mg, 1.0 equivalent) as prepared in Example 7 was dissolved in toluene (0.09 M) and DMF (0.26 M), and to which acetic acid (2.0 equivalents), and ethyl 4,4,4-triethoxybutanoate (4.0 equivalents) were added and the reaction mixture was heated to 85° C. for 9 hrs. The reaction mixture was then partitioned between ethyl acetate and water and the separated organics was washed with brine and dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by SiO2 chromatography (5%-10% MeOH/CH2Cl2 gradient) to afford ethyl 3-(8-(2-(3-ethylureido)benzo[b]thiophene-3-carbonyl)-4-oxo-1,3,8-triazaspiro[4.5]dec-1-en-2-yl)propanoate (10, 65%). Two rotamers observed (ratio 1.3:1).

後処理

  1. customThe reaction mixture was then partitioned between ethyl acetate and water
  2. washthe separated organics was washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by SiO2 chromatography (5%-10% MeOH/CH2Cl2 gradient)

出典と根拠

ORDレコード
ord-5c8e6aa685ce424e95a19a6b0660754c
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07981904B2

反応ノート

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