1-Hydroxybenzotriazole → HCID 178482473, 화합물

HRID 1620506노트

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HRID 1620506 반응식
[CH3:1][C:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][C:3]=1[C:11]([OH:13])=O.ON1C2C=CC=CC=2N=N1.Cl.C(N=C=NCCCN(C)C)C.Cl.Cl.[CH3:38][NH:39][C:40]1=[N:41][C:42](=[O:52])[S:43]/[C:44]/1=[CH:45]\[CH:46]1[CH2:51][CH2:50][NH:49][CH2:48][CH2:47]1>CN(C)C=O.O.C(N(CC)CC)C>[CH3:38][NH:39][C:40]1=[N:41][C:42](=[O:52])[S:43]/[C:44]/1=[CH:45]\[CH:46]1[CH2:51][CH2:50][N:49]([C:11]([C:3]2[O:4][C:5]3[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=3[C:2]=2[CH3:1])=[O:13])[CH2:48][CH2:47]1

참가 물질

8

반응물 4

HCID 757711-HydroxybenzotriazoleHCID 6005913-Methyl-1-benzofuran-2-carboxylic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 178482469HCID 178482469, 화합물

생성물 1

HCID 178482473HCID 178482473, 화합물수율 50.4%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8471Triethylamine용매

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온도
0 °C

실험 절차

To a solution of 3-methyl-1-benzofuran-2-carboxylic acid (19.4 mg) in N,N-dimethylformamide (1 mL) were added 1-hydroxybenzotriazole (16.2 mg) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (23 mg), and the mixture was stirred at 0° C. for 5 min. To the reaction mixture were added triethylamine (0.28 mL) and (5Z)-4-(methylamino)-5-(piperidin-4-ylmethylidene)-1,3-thiazol-2(5H)-one dihydrochloride (29.8 mg), and the mixture was further stirred at room temperature for 5 hr. Water was added to the reaction mixture, and the precipitate was collected by filtration, and washed with water and diisopropyl ether to give the title compound (19.3 mg).

후처리

  1. stirringthe mixture was further stirred at room temperature for 5 hr
  2. filtrationthe precipitate was collected by filtration
  3. washwashed with water and diisopropyl ether

출처 및 근거

ORD 기록
ord-f7f2c43d813340dab9155750bcee77d6
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772277B2

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