Hydrazine hydrate (1:1) → HCID 178473791、化合物

HRID 57288ノート

反応式

HRID 57288 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([C:10](OS(C2C=CC(C)=CC=2)(=O)=O)=[C:11]([C:14]2[S:15][C:16]3[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=3[N:18]=2)[C:12]#[N:13])[CH2:6][CH2:5]1)(=O)[CH3:2].[OH2:34].[NH2:35][NH2:36]>CO>[NH2:13][C:12]1[NH:36][N:35]=[C:10]([CH:7]2[CH2:8][CH2:9][N:4]([C:1](=[O:34])[CH3:2])[CH2:5][CH2:6]2)[C:11]=1[C:14]1[S:15][C:16]2[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=2[N:18]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 86608764HCID 86608764、化合物

生成物 1

HCID 178473791HCID 178473791、化合物収率 55%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of the above prepared toluene-4-sulfonic acid 1-(1-acetylpiperidin-4-yl)-2-benzothiazol-2-yl-2-cyanovinyl ester (140 mg, 0.29 mmol) and hydrazine hydrate (25 mg, 0.5 mmol) in methanol was refluxed overnight. The solvent was evaporated and the residue was purified by flash column chromatography eluting with CH2Cl2:MeOH=20:1 to yield 54 mg (55%) of 1-[4-(5-amino-4-benzothiazol-2-yl-1H-pyrazol-3-yl)-piperidin-1-yl]-ethanone. MS (ES+): 342.1 (M+1, 100%).

後処理

  1. additionA mixture of the
  2. temperaturewas refluxed overnight
  3. customThe solvent was evaporated
  4. customthe residue was purified by flash column chromatography
  5. washeluting with CH2Cl2

出典と根拠

ORDレコード
ord-d8224a17ed4940e2b0dc0b8c5afd2389
出典データセット
uspto-grants-2016_09
特許番号
US09434720B2

反応ノート

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