Triethylamine → HCID 21071758, 화합물

HRID 1372473노트

반응식

HRID 1372473 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 21071758HCID 21071758, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6969b2944f9e4114b04c0ee3ac839848
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07157490B2

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