Triethylamine → HCID 24751933, 화합물

HRID 252243노트

반응식

HRID 252243 반응식
[N-]=C=O.[C:4]1([CH3:17])[CH:9]=[CH:8][C:7]([S:10]([NH:13][C:14]([NH2:16])=[O:15])(=[O:12])=[O:11])=[CH:6][CH:5]=1.Cl.N[C:20]1[S:21][C:22]([Br:25])=[CH:23][N:24]=1.C(N(CC)CC)C>C(Cl)Cl>[Br:25][C:22]1[S:21][C:20]([NH:16][C:14]([NH:13][S:10]([C:7]2[CH:6]=[CH:5][C:4]([CH3:17])=[CH:9][CH:8]=2)(=[O:11])=[O:12])=[O:15])=[N:24][CH:23]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 221703925-Bromo-1,3-thiazol-2-amine--hydrogen chloride (1/1)HCID 86616716Toluene-4-sulfonylurea isocyanate

생성물 1

HCID 24751933HCID 24751933, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of toluene-4-sulfonylurea isocyanate (2.6 g, 13 mmol) in CH2Cl2 (10 ml) was added slowly to a mixture containing 2-amino-5-bromothiazole hydrochloride (3.4 g, 13 mmol) and triethylamine (5.4 ml, 39 mmol) in CH2Cl2 (60 ml) under an argon atmosphere and stirred overnight at rt. The reaction mixture was concentrated under reduce pressure, diluted with ethyl acetate and washed with NaHCO3 (half sat. 3×), 5% KHSO4/10% K2SO4, water, NaCl sat., dried (MgSO4.2H2O), filtered and concentrated under reduced pressure. Recrystallization from MeOH/water yielded a beige solid: 2.8 g (58%), MS: m/e 376.1 (MH+).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. additiondiluted with ethyl acetate
  3. washwashed with NaHCO3 (half sat. 3×), 5% KHSO4/10% K2SO4, water, NaCl sat.
  4. dry with materialdried (MgSO4.2H2O)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customRecrystallization from MeOH/water
  8. customyielded a beige solid

출처 및 근거

ORD 기록
ord-de66dd01d4764801b519b2e2fd4230d7
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07868030B2

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