Triethylamine → HCID 68842437、化合物

HRID 660599ノート

反応式

HRID 660599 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[C:13](I)[CH:12]=[CH:11][C:10]=1[N:16]1[S:20](=[O:22])(=[O:21])[NH:19][C:18](=[O:23])[CH2:17]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:24]([O:28][C:29](=[O:32])[CH:30]=[CH2:31])([CH3:27])([CH3:26])[CH3:25].C(N(CC)CC)C>C(#N)C.CC([O-])=O.CC([O-])=O.[Pd+2]>[C:24]([O:28][C:29](=[O:32])/[CH:30]=[CH:31]/[C:13]1[CH:12]=[CH:11][C:10]([N:16]2[CH2:17][C:18](=[O:23])[NH:19][S:20]2(=[O:22])=[O:21])=[C:9]([O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH:14]=1)([CH3:27])([CH3:26])[CH3:25]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 15458tert-Butyl acrylateHCID 688386435-(2-Benzyloxy-4-iodophenyl)-1,1-dioxo-1,2,5-thiadiazolidin-3-one

生成物 1

HCID 68842437HCID 68842437、化合物

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 6342Acetonitrile溶媒

反応条件

温度
100 °C

実験手順

To a mixture of 5-(2-benzyloxy-4-iodophenyl)-1,1-dioxo-1,2,5-thiadiazolidin-3-one (2.0 g, 4.49 mmol), Pd(OAc)2 (100 mg) and acrylic acid t-butyl ester (0.78 mL, 5.8 mmol) in acetonitrile (15 mL) in a pressure vessel is added triethylamine (3.13, 22.5 mmol) and the mixture is stirred at 100° C. for 6 h. The solution is filtered through Celite, washed with acetonitrile and concentrated to give the title compound. This is used directly in the next step.

後処理

  1. filtrationThe solution is filtered through Celite
  2. washwashed with acetonitrile
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-c8328f7d3c6341748f838b79f5dd451e
出典データセット
uspto-grants-2011_12
特許番号
US08084448B2

反応ノート

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