Tributylvinyltin → HCID 54101958、化合物

HRID 354050

反応式

HRID 354050 の反応式
[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]

参加物

5

反応物 2

HCID 81998TributylvinyltinHCID 54481034HCID 54481034、化合物

生成物 1

HCID 54101958HCID 54101958、化合物

試薬・触媒・溶媒 2

HCID 84124Bis(triphenylphosphine)palladium chloride触媒HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  1. customEvaporation and chromatography

出典と根拠

ORDレコード
ord-cb46442e978e4c5ea6ef46da9b68f99c
出典データセット
uspto-grants-2004_06
特許番号
US06756360B1

関連ノート

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