1-Hydroxybenzotriazole → HCID 46927104, 화합물

HRID 1891114노트

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HRID 1891114 반응식
[CH3:1][N:2]1[C:7]2=[CH:8][S:9][C:10](C)=[C:6]2[C:5](=[O:12])[N:4]([CH3:13])[C:3]1=[O:14].[Br:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]2[S:26][C:25]([NH2:27])=[N:24][N:23]=2)=[CH:18][CH:17]=1.CCN=C=NC[CH2:34][CH2:35]N(C)C.Cl.C1C=CC2N([OH:49])N=NC=2C=1>CN(C1C=CN=CC=1)C.ClCCCl>[Br:15][C:16]1[CH:17]=[CH:18][C:19]([C:22]2[S:26][C:25]([NH:27][C:34](=[O:49])[CH2:35][C:7]3[C:6]4[C:5](=[O:12])[N:4]([CH3:13])[C:3](=[O:14])[N:2]([CH3:1])[C:10]=4[S:9][CH:8]=3)=[N:24][N:23]=2)=[CH:20][CH:21]=1

참가 물질

7

반응물 4

HCID 757711-HydroxybenzotriazoleHCID 5542155-(4-Bromophenyl)-1,3,4-thiadiazol-2-amineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 710080931,3,5-trimethylthieno[3,4-d]pyrimidine-2,4(1H,3H)-dione

생성물 1

HCID 46927104HCID 46927104, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 111,2-Dichloroethane용매

실험 절차

The title compound was prepared according to the general procedure (Method A) by coupling Intermediate 1 (100 mg, 0.393 mmol) with 5-(4-bromophenyl)-1,3,4-thiadiazol-2-amine (101 mg, 0.393 mmol) in the presence of EDCI hydrochloride (90 mg, 0.472 mmol), HOBt (16 mg, 0.118 mmol) and DMAP (5 mg, 0.039 mmol) in 1,2 dichloroethane (4 ml) to give 45 mg of the product as an off-white solid; 1H NMR (300 MHz, DMSO-d6) δ 3.18 (s, 3H), 3.47 (s, 3H), 4.11 (s, 2H), 7.09 (s, 1H), 7.72 (d, J=8.4 Hz, 2H), 7.87 (d, J=8.1 Hz, 2H), 12.85 (br s, 1H); APCI-MS (m/z) 493.93 (M+H)+.

출처 및 근거

ORD 기록
ord-a38ee5881fff4773bda18ae744aa6ed5
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507503B2

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