1,2-Dichloroethane → HCID 178420052, 화합물

HRID 1678772노트

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HRID 1678772 반응식
[NH:1]([C:3]1[N:12]=[CH:11][CH:10]=[C:9]2[C:4]=1[CH:5]=[C:6]([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)[C:7]([C:13]1[CH:18]=[CH:17][C:16]([CH2:19][N:20]3[CH2:25][CH2:24][CH:23]([C:26]4[NH:30][C:29]([C:31]5[N:36]=[CH:35][CH:34]=[CH:33][N:32]=5)=[N:28][N:27]=4)[CH2:22][CH2:21]3)=[CH:15][CH:14]=1)=[N:8]2)[NH2:2].C1C=C[C:46]2[N:51](O)[N:50]=[N:49][C:47]=2[CH:48]=1.N1C=C(C(O)=O)N=N1.CCN(C(C)C)C(C)C.C(Cl)CCl>CN(C=O)C.C(O)(=O)C>[C:37]1([C:6]2[C:7]([C:13]3[CH:18]=[CH:17][C:16]([CH2:19][N:20]4[CH2:21][CH2:22][CH:23]([C:26]5[NH:30][C:29]([C:31]6[N:36]=[CH:35][CH:34]=[CH:33][N:32]=6)=[N:28][N:27]=5)[CH2:24][CH2:25]4)=[CH:15][CH:14]=3)=[N:8][C:9]3[CH:10]=[CH:11][N:12]4[C:48]([C:47]5[N:49]=[N:50][NH:51][CH:46]=5)=[N:2][N:1]=[C:3]4[C:4]=3[CH:5]=2)[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=1

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 1401204-Carboxy-1,2,3-triazoleHCID 178514342HCID 178514342, 화합물

생성물 1

HCID 178420052HCID 178420052, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 6228Dimethylformamide용매

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온도
80 °C

실험 절차

To a stirred solution of 11-3 (0.2 g, 0.36 mMol), HOBT (0.05 g, 0.4 mMol), and 1H-1,2,3-triazole-4-carboxylic acid (0.05 g, 0.4 mMol) in anhydrous DMF (2 mL) was added DIEA (0.18 mL, 1.1 mMol) followed by EDC (0.08 g, 0.4 mMol). The solution was heated in the microwave reactor for 30 minutes at 80° C. Solution was then treated with 0.5 mL of acetic acid and was heated to 80° C. in the microwave reactor for 10 min. Upon cooling to room temperature, the solution was passed through a syringe filter and purified on a C18 reverse phase HPLC to give 11-4 as a solid. Mass (M+1) calculated: 632.2742 observed: 632.274

후처리

  1. temperaturewas heated to 80° C. in the microwave reactor for 10 min
  2. temperatureUpon cooling to room temperature
  3. customthe solution was passed through a syringe
  4. filtrationfilter
  5. custompurified on a C18 reverse phase HPLC

출처 및 근거

ORD 기록
ord-4ef5b63c404449e7b83e392c291c1f8d
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08008317B2

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