Triethylamine → HCID 24751933、化合物

HRID 252243ノート

反応式

HRID 252243 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 24751933HCID 24751933、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-de66dd01d4764801b519b2e2fd4230d7
出典データセット
uspto-grants-2011_01
特許番号
US07868030B2

反応ノート

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