Tributylvinyltin → HCID 54101958, 화합물

HRID 354050

반응식

HRID 354050 반응식
[CH2:1]([O:3][P:4]([CH2:9][O:10][C:11]1[CH:16]=[CH:15][C:14](OC)=[CH:13][C:12]=1[N+:19]([O-:21])=[O:20])([O:6][CH2:7][CH3:8])=[O:5])[CH3:2].[CH2:22]([Sn](CCCC)(CCCC)C=C)[CH2:23]CC>CN(C=O)C.[Cl-].[Cl-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Pd+2]>[CH2:7]([O:6][P:4]([CH2:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([CH:22]=[CH2:23])=[CH:13][C:12]=1[N+:19]([O-:21])=[O:20])([O:3][CH2:1][CH3:2])=[O:5])[CH3:8]

참가 물질

5

반응물 2

HCID 81998TributylvinyltinHCID 54481034HCID 54481034, 화합물

생성물 1

HCID 54101958HCID 54101958, 화합물

시약·촉매·용매 2

HCID 84124Bis(triphenylphosphine)palladium chloride촉매HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

A solution of 2-diethylphosphonomethyloxy-5-bromonitrobenzene (1 mmole, prepared as in Example 37, Step A) in DMF (5 mL) was treated with tributyl(vinyl)tin (1.2 mmole) and palladium bis(triphenylphosphine) dichloride (0.1 mmole), and the mixture was heated at 60° C. under nitrogen for 6 h. Evaporation and chromatography gave 2-diethylphosphonomethyloxy-5-vinylnitrobenzene as an oil which was subjected to Step B of Example 38, Step B of Example 36, and Step D of Example 34 to give 2-amino-7-ethyl-6-thiocyano-4-phosphonomethoxybenzothiazole (41.1). mp >167° C.(dec.). Anal. Calcd. for C11H12N3O4PS2: C:38.26; H:3.50; N:12.17. Found: C:37.87; H:3.47; N: 11.93.

후처리

  1. customEvaporation and chromatography

출처 및 근거

ORD 기록
ord-cb46442e978e4c5ea6ef46da9b68f99c
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06756360B1

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