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1,2-Dichloroethane → HCID 9912198、化合物

HRID 1584277
ノート
印刷プレビュー

反応式

HRID 1584277 の反応式
[CH2:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][C@@H:3]([CH2:11][N:12]2[C:16]([CH2:17][C:18]3[CH:25]=[CH:24][C:21]([C:22]#[N:23])=[CH:20][CH:19]=3)=[CH:15][N:14]=[CH:13]2)[NH:2]1.[CH3:26][O:27][C:28]1[CH:29]=[C:30]([CH:34]=[CH:35][CH:36]=1)[C:31](O)=[O:32].ON1C2C=CC=CC=2N=N1.C(Cl)CCl.CN1CCOCC1>CN(C=O)C>[CH3:26][O:27][C:28]1[CH:29]=[C:30]([CH:34]=[CH:35][CH:36]=1)[C:31]([N:2]1[C@H:3]([CH2:11][N:12]2[C:16]([CH2:17][C:18]3[CH:19]=[CH:20][C:21]([C:22]#[N:23])=[CH:24][CH:25]=3)=[CH:15][N:14]=[CH:13]2)[CH2:4][C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH2:1]1)=[O:32]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 111,2-DichloroethaneHCID 79724-MethylmorpholineHCID 114613-Methoxybenzoic AcidHCID 757711-HydroxybenzotriazoleHCID 54328958HCID 54328958、化合物

生成物 1

HCID 9912198HCID 9912198、化合物

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
25 °C

実験手順

A mixture of 4-{3-[(S)-1,2,3,4-tetrahydro-isoquinolin-3-yl-methyl]-3H-imidazol-4-yl-methyl}-benzonitrile (0.16 g, 0.487 mmol), 3-methoxybenzoic acid (0.074 g, 0.487 mmol), 1-hydroxybenzotriazole (0.075 g, 0.487 mmol), EDC (0.093 g, 0.487 mmol) and N-methylmorpholine (0.2 ml, 1.95 mmol) in 5 ml DMF was stirred for 18 hr at 25° C. The solvent was removed in vacuo. The residue was partitioned between ethyl acetate and saturated sodium bicarbonate. The ethyl acetate layer was dried with saturated sodium chloride and magnesium sulfate. Evaporation in vacuo of the ethyl acetate layer yielded the crude product. Purification was done on silica gel using methylene chloride:methanol:amonia hydroxide 98:2:0.2 and yielded the title compound.

後処理

  1. customThe solvent was removed in vacuo
  2. customThe residue was partitioned between ethyl acetate and saturated sodium bicarbonate
  3. dry with materialThe ethyl acetate layer was dried with saturated sodium chloride and magnesium sulfate
  4. customEvaporation in vacuo of the ethyl acetate layer
  5. customyielded the crude product
  6. customPurification

出典と根拠

ORDレコード
ord-582b6081bc7e4b3e9c7f8a40d5853c9a
出典データセット
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05932590

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート