1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 2,6-Diamino-nicotinic acid N'-(2-(4-benzyloxy-phenyl)-acetyl)-hydrazide

HRID 1927232노트

반응식

HRID 1927232 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][C:16]([NH:18][NH2:19])=[O:17])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:20][C:21]1[N:29]=[C:28]([NH2:30])[CH:27]=[CH:26][C:22]=1[C:23](O)=[O:24].C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C>O.C(N(CC)CC)C.CN(C=O)C>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][C:16]([NH:18][NH:19][C:23](=[O:24])[C:22]2[CH:26]=[CH:27][C:28]([NH2:30])=[N:29][C:21]=2[NH2:20])=[O:17])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

8

반응물 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 189772452,6-Diaminonicotinic acidHCID 59287387(4-Benzyloxy-phenyl)-acetic acid hydrazide

생성물 1

HCID 592873832,6-Diamino-nicotinic acid N'-(2-(4-benzyloxy-phenyl)-acetyl)-hydrazide수율 66.9%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8471Triethylamine용매

실험 절차

To a solution of DMF (1 mL) of (4-benzyloxy-phenyl)-acetic acid hydrazide (46 mg) described in Manufacturing Example 8-1 were added triethylamine (0.10 mL), 2,6-diamino-nicotinic acid (30 mg) described in Manufacturing Example 10-2-4, HOBt (27 mg), and WSC (41 mg), which was stirred overnight at the same temperature. Water was added to the reaction solution, and the precipitated solids were filtered off to obtain the titled compound (47 mg) as a crude form. This compound was used directly as a crude form in the subsequent reaction.

후처리

  1. filtrationthe precipitated solids were filtered off

출처 및 근거

ORD 기록
ord-fcc31a2ab1984755b1b53c0f3dec231f
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08183264B2

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