O-Phenylenediamine → HCID 44540344, 화합물

HRID 1926198노트

반응식

HRID 1926198 반응식
[Cl:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][C:8]([Cl:15])=[CH:9][CH:10]=3)[C:5](=[CH:16][C:17]([NH:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][C:25](O)=[O:26])=[O:18])[C:4]=2[CH:3]=1.Cl.C(N=C=NCCCN(C)C)C.O[C:41]1[C:49]2[N:48]=N[NH:46][C:45]=2[CH:44]=[CH:43][CH:42]=1.C(N(CC)CC)C.C1(N)C=CC=CC=1N>[Cl-].[Na+].O.CN(C=O)C>[Cl:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][C:8]([Cl:15])=[CH:9][CH:10]=3)[C:5](=[CH:16][C:17]([NH:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][C:25]([NH:46][C:45]3[CH:44]=[CH:43][CH:42]=[CH:41][C:49]=3[NH2:48])=[O:26])=[O:18])[C:4]=2[CH:3]=1

참가 물질

8

반응물 5

HCID 7243O-PhenylenediamineHCID 8471TriethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 67520676HCID 67520676, 화합물HCID 178418300HCID 178418300, 화합물

생성물 1

HCID 44540344HCID 44540344, 화합물수율 71%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 57417360Sodium chloride; water용매

실험 절차

6-(2-(2,7-dichloro-9H-fluoren-9-ylidene)acetamido)hexanoic acid (403 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 (351 mg, 71% yield) as a brown solid. LC-MS (m/z) 494 (M+1).

후처리

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

출처 및 근거

ORD 기록
ord-35b226b016864575bbba4d30ea85890f
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178577B2

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