Benzoic Acid → HCID 21264391、化合物

HRID 567098ノート

反応式

HRID 567098 の反応式
[C:1](O)(=[O:8])[C:2]1[CH:7]=[CH:6]C=[CH:4][CH:3]=1.[OH:10]N1C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC.[CH2:32]([N:34]([CH2:37][CH3:38])[CH2:35][CH3:36])[CH3:33].[Cl:39][C:40]1[CH:45]=[CH:44][C:43]([CH:46]2[C:51]3[CH:52]=[CH:53][S:54][C:50]=3[CH2:49][CH2:48][NH:47]2)=[CH:42][CH:41]=1.CN(C)[CH:57]=[O:58]>C(OCC)(=O)C.O>[Cl:39][C:40]1[CH:41]=[CH:42][C:43]([CH:46]2[C:51]3[CH:52]=[CH:53][S:54][C:50]=3[CH2:49][CH2:48][N:47]2[C:1]([C:2]2[CH:7]=[CH:6][C:57]([O:58][CH2:33][CH2:32][N:34]3[CH2:37][CH2:38][O:10][CH2:36][CH2:35]3)=[CH:4][CH:3]=2)=[O:8])=[CH:44][CH:45]=1

参加物

9

反応物 6

HCID 243Benzoic AcidHCID 6228DimethylformamideHCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27392694-(4-Chlorophenyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine

生成物 1

HCID 21264391HCID 21264391、化合物収率 66%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

The above benzoic acid (111 mg, 0.38 mmoles) was suspended in N,N-dimethylformamide (1 mL). 1-Hydroxybenzotriazole (55 mg, 0.42 mmoles), N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (79 mg, 0.42 mmoles), and triethylamine (106 μL, 0.76 mmoles) were added and the resulting mixture was shaken at 1000 rpm for 1.5 hour. 4-(4-Chlorophenyl)-4,5,6,7-tetrahydro-thieno[3,2-c]pyridine (100 mg, 0.38 mmoles) was added and the resulting mixture was shaken at 1000 rpm for 3 hours. Water (2 mL) and ethyl acetate (1 mL) were added and the resulting mixture was shaken at 1000 rpm for 15 minutes, The organic phase was evaporated to afford 122 mg (66%) of the title compound as an oil.

後処理

  1. stirringthe resulting mixture was shaken at 1000 rpm for 3 hours
  2. stirringthe resulting mixture was shaken at 1000 rpm for 15 minutes
  3. customThe organic phase was evaporated

出典と根拠

ORDレコード
ord-77f0b759333f480e8ab6755fabad7b13
出典データセット
uspto-grants-2001_01
特許番号
US06177443B1

反応ノート

読み込み中…