Triethylamine → HCID 21071758、化合物

HRID 1372473ノート

反応式

HRID 1372473 の反応式
C1N=CN([C:6](N2C=NC=C2)=[O:7])C=1.[I:13][C:14]1[CH:15]=[C:16]([CH:21]=[CH:22][CH:23]=1)[C:17]([NH:19][NH2:20])=[O:18].C(N(CC)CC)C>C1COCC1>[I:13][C:14]1[CH:15]=[C:16]([C:17]2[O:18][C:6](=[O:7])[NH:20][N:19]=2)[CH:21]=[CH:22][CH:23]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 6157743-Iodobenzohydrazide

生成物 1

HCID 21071758HCID 21071758、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of N,N-carbonyldiimidazole (800 mg, 5.0 mmol) in 5 mL of dry THF was added dropwise to an ice-cold solution of the product from Step A (1.048 g, 4.0 mmol) and triethylamine (0.60 mL, 4.0 mmol) in 12 mL of dry THF. The resultant mixture was allowed to warm to room temperature overnight, and was then concentrated under reduced pressure. The residue was partitioned between diethyl ether and water, and the ether layer was washed sequentially with 5% aqueous hydrochloric acid, saturated aqueous sodium bicarbonate solution, and saturated aqueous brine, dried (magnesium sulfate), and concentrated under reduced pressure to afford a white powder. Recrystallization from ethyl acetate-hexanes afforded the title compound as a fluffy white solid. LC/MS 289.2 (M+1).

後処理

  1. concentrationwas then concentrated under reduced pressure
  2. customThe residue was partitioned between diethyl ether and water
  3. washthe ether layer was washed sequentially with 5% aqueous hydrochloric acid, saturated aqueous sodium bicarbonate solution, and saturated aqueous brine
  4. dry with materialdried (magnesium sulfate)
  5. concentrationconcentrated under reduced pressure
  6. customto afford a white powder
  7. customRecrystallization from ethyl acetate-hexanes

出典と根拠

ORDレコード
ord-6969b2944f9e4114b04c0ee3ac839848
出典データセット
uspto-grants-2007_01
特許番号
US07157490B2

反応ノート

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