1,2-Dichloroethane → HCID 178420052、化合物

HRID 1678772ノート

反応式

HRID 1678772 の反応式
[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

参加物

8

反応物 5

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

生成物 1

HCID 178420052HCID 178420052、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-4ef5b63c404449e7b83e392c291c1f8d
出典データセット
uspto-grants-2011_08
特許番号
US08008317B2

反応ノート

読み込み中…