O-Phenylenediamine → HCID 44540433、化合物

HRID 1926200ノート

反応式

HRID 1926200 の反応式
[N+:1]([C:4]1[CH:16]=[CH:15][C:14]2[C:13]3[C:8](=[CH:9][C:10]([N+:17]([O-:19])=[O:18])=[CH:11][CH:12]=3)[C:7](=[CH:20][C:21]([NH:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][C:29]([OH:31])=O)=[O:22])[C:6]=2[CH:5]=1)([O-:3])=[O:2].Cl.C(N=C=NCCCN(C)C)C.O[C:45]1[C:53]2[N:52]=N[NH:50][C:49]=2[CH:48]=[CH:47][CH:46]=1.C(N(CC)CC)C.C1(N)C=CC=CC=1N>[Cl-].[Na+].O.CN(C=O)C>[N+:1]([C:4]1[CH:16]=[CH:15][C:14]2[C:13]3[C:8](=[CH:9][C:10]([N+:17]([O-:19])=[O:18])=[CH:11][CH:12]=3)[C:7](=[CH:20][C:21]([NH:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][C:29]([NH:50][C:49]3[CH:48]=[CH:47][CH:46]=[CH:45][C:53]=3[NH2:52])=[O:31])=[O:22])[C:6]=2[CH:5]=1)([O-:3])=[O:2]

参加物

8

反応物 5

HCID 7243O-PhenylenediamineHCID 8471TriethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 86636548HCID 86636548、化合物HCID 178418300HCID 178418300、化合物

生成物 1

HCID 44540433HCID 44540433、化合物収率 84%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

6-(2-(2,7-dinitro-9H-fluoren-9-ylidene)acetamido)hexanoic acid (425 mg, 1 mmol), and 8 ml of DMF were stirred at room temperature while 1-Ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (394 mg, 2 mmol), hydroxy-benzotriazole (162 mg, 1.2 mmol), triethylamine (404 mg, 4 mmol) and o-phenylenediamine (432 mg, 4 mmol) were added. The mixture was stirred for 24 hours at room temperature. The mixture was diluted with 400 mL of brine. The solids were collected by vacuum filtration, washed with water and dried under vacuum to give the title compound (433 mg, 84% yield) as a brown solid. LC-MS (m/z) 516 (M+1).

後処理

  1. additionwere added
  2. filtrationThe solids were collected by vacuum filtration
  3. washwashed with water
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-52b3f116d3504dd7aa3bc9903b84b474
出典データセット
uspto-grants-2012_05
特許番号
US08178577B2

反応ノート

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