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1-Hydroxybenzotriazole → N-(6-Cyano-1H-benzimidazol-2-yl)-2-(3-fluorophenyl)cyclopropanecarboxamide

HRID 1403072
ノート
印刷プレビュー

反応式

HRID 1403072 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:8]2[CH2:10][CH:9]2[C:11]([OH:13])=O)[CH:5]=[CH:6][CH:7]=1.Cl.C(N=C=NCCCN(C)C)C.ON1C2C=CC=CC=2N=N1.Cl.[NH2:37][C:38]1[NH:39][C:40]2[CH:46]=[C:45]([C:47]#[N:48])[CH:44]=[CH:43][C:41]=2[N:42]=1>CN(C=O)C>[C:47]([C:45]1[CH:44]=[CH:43][C:41]2[N:42]=[C:38]([NH:37][C:11]([CH:9]3[CH2:10][CH:8]3[C:4]3[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[CH:3]=3)=[O:13])[NH:39][C:40]=2[CH:46]=1)#[N:48]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 218646592-(3-Fluorophenyl)cyclopropanecarboxylic acidHCID 867295832-Amino-3H-benzoimidazole-5-carbonitril hydrochloride

生成物 1

HCID 71513846N-(6-Cyano-1H-benzimidazol-2-yl)-2-(3-fluorophenyl)cyclopropanecarboxamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2-(3-Fluoro-phenyl)-cyclopropanecarboxylic acid 2 (90 mg, 0.50 mmol) was dissolved in 10 ml DMF. 115 mg (0.6 mmol) 1-Ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (EDC) and 81 mg (0.6 mmol) 1-Hydroxybenzotriazole (HOBT) were added. The mixture was stirred for 30 min at room temperature (RT). Then 97 mg (0.5 mmol) 2-Amino-3H-benzoimidazole-5-carbonitril hydrochloride 1 were added to the mixture, which was stirred for 16 h at RT. After removing the solvent in vacuo, 20 ml water were added, whereupon the mixture was extracted 3 times with 50 ml acetic acid ethylester. The organic phases were combined, dried with sodium sulfate, and evaporated to dryness. The residue was separated via preparative HPLC. The resulting clean fractions were concentrated and lyophilized. 91 mg (57%) of a colorless, amorphous solid 3 were obtained.

後処理

  1. stirringwas stirred for 16 h at RT
  2. customAfter removing the solvent in vacuo, 20 ml water
  3. additionwere added, whereupon the mixture
  4. extractionwas extracted 3 times with 50 ml acetic acid ethylester
  5. dry with materialdried with sodium sulfate
  6. customevaporated to dryness
  7. customThe residue was separated via preparative HPLC
  8. concentrationThe resulting clean fractions were concentrated

出典と根拠

ORDレコード
ord-ddf8606d781d421da62a240339fd63e4
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08912202B2

反応ノート

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