Triethylamine → 5-(2-(9H-fluoren-9-ylidene)acetamido)pentanoic acid methyl ester

HRID 1926186노트

반응식

HRID 1926186 반응식
[CH:1]1[C:13]2[C:12](=[CH:14][C:15](O)=[O:16])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.Cl.C(N=C=NCCCN(C)C)C.OC1C2N=NNC=2C=CC=1.C(N(CC)CC)C.Cl.[CH3:48][O:49][C:50](=[O:56])[CH2:51][CH2:52][CH2:53][CH2:54][NH2:55]>[Cl-].[Na+].O.CN(C=O)C>[CH3:48][O:49][C:50](=[O:56])[CH2:51][CH2:52][CH2:53][CH2:54][NH:55][C:15](=[O:16])[CH:14]=[C:12]1[C:13]2[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=2[C:6]2[C:11]1=[CH:10][CH:9]=[CH:8][CH:7]=2

참가 물질

8

반응물 5

HCID 8471TriethylamineHCID 967929H-Fluoren-9-ylideneacetic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 13672034Methyl 5-aminopentanoate hydrochlorideHCID 178418300HCID 178418300, 화합물

생성물 1

HCID 579720535-(2-(9H-fluoren-9-ylidene)acetamido)pentanoic acid methyl ester수율 82.9%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 57417360Sodium chloride; water용매

실험 절차

2-(9H-fluoren-9-ylidene)acetic acid (222 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), hydroxybenzo-triazole (162 mg, 1.2 mmol), triethylamine (404 mg, 4 mmol) and 5-aminovaleric acid methyl ester hydrochloride (202 mg, 1.2 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 (278 mg, 68% yield) as a white solid. LC-MS (m/z) 336 (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-a479601e4d144f0a8d5655deb5928ce7
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178577B2

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