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1,2-Dichloroethane → HCID 58979489、化合物

HRID 1181093
ノート
印刷プレビュー

反応式

HRID 1181093 の反応式
[CH2:1]([O:3][C:4](=[O:27])[C:5]([O:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:11][C:10]=1[CH2:23][C:24](O)=[O:25])([CH3:7])[CH3:6])[CH3:2].[Cl-].[NH4+].C(Cl)CCl.O.O[N:36]1C2C=CC=CC=2N=N1.C(N(C(C)C)C(C)C)C>CN(C=O)C>[CH2:1]([O:3][C:4](=[O:27])[C:5]([O:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:11][C:10]=1[CH2:23][C:24](=[O:25])[NH2:36])([CH3:7])[CH3:6])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 111,2-DichloroethaneHCID 25517Ammonium ChlorideHCID 81531DiisopropylethylamineHCID 27960291-Hydroxybenzotriazole hydrateHCID 58979077HCID 58979077、化合物

生成物 1

HCID 58979489HCID 58979489、化合物収率 86.4%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

2-(4-Benzyloxy-2-carboxymethyl-phenoxy)-2-methyl-propionic acid ethyl ester (500 mg, 1.34 mmol), ammonium chloride (108 mg, 2.02 mmol), EDC (3.86 mg, 2.01 mmol), and N-hydroxybenzotriazole hydrate (272 mg, 2.01 mmol) were combined in a flask and diluted with DMF (5 mL). Ethyl diisopropyl amine (0.70 mL, 4.0 mmol) was added. The solution was stirred for 18 h and partitioned between EtOAc (25 mL) and 1N HCl (10 mL). The organic layer was washed with saturated NaHCO3 solution (10 mL) then brine (10 mL), dried (Na2SO4), and concentrated. The crude product was purified by radial chromatography (hexanes/EtOAc 1/2 to 1/4) to give the title compound (430 mg, 86%).

後処理

  1. custompartitioned between EtOAc (25 mL) and 1N HCl (10 mL)
  2. washThe organic layer was washed with saturated NaHCO3 solution (10 mL)
  3. dry with materialbrine (10 mL), dried (Na2SO4)
  4. concentrationconcentrated
  5. customThe crude product was purified by radial chromatography (hexanes/EtOAc 1/2 to 1/4)

出典と根拠

ORDレコード
ord-7b3951cbdb05470d8853b0ae52fa084b
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07282501B2

反応ノート

読み込み中…

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