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Dabco → HCID 54057117、化合物

HRID 1973398
ノート
印刷プレビュー

反応式

HRID 1973398 の反応式
[OH:1][C:2]1[C:10]2[C:6](=[CH:7][S:8][N:9]=2)[CH:5]=[CH:4][CH:3]=1.C1N2CCN(CC2)C1.CCCCC(C([O-])=O)CC.CCCCC(C([O-])=O)CC.[Sn+2].[CH3:40][N:41]=[C:42]=[O:43]>C1C=CC=CC=1>[N:9]1[S:8][CH:7]=[C:6]2[CH:5]=[CH:4][CH:3]=[C:2]([O:1][C:42](=[O:43])[NH:41][CH3:40])[C:10]=12
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 9237DabcoHCID 93182-ethylhexanoic acid tin(II) saltHCID 12228Methyl IsocyanateHCID 214914432,1-Benzothiazol-7-ol

生成物 1

HCID 54057117HCID 54057117、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To a solution of 2.0 g. 7-hydroxy-2,1-benzisothiazole, 40 ml. dry benzene, and catalytic amounts of triethylenediamine and stannous octoate was added 2.5 g. methylisocyanate. After about five minutes at room temperature, yellow solid carbamate product crystallized from solution. The mixture was allowed to stand at room temperature overnight, then solvent and excess methylisocyanate were removed by evaporation on a rotatory evaporator. The solid residue was washed with hot hexane and isolated by suction filtration to give 2.6 g. yellow, microcrystalline 2,1-benzisothiazol-7-yl N-methylcarbamate, mp. 145°-148° (dec.) after recrystallization from benzene. This structure was confirmed by ir and nmr. The insecticidal activity of this material was determined exactly as described in Example 12, whereby 2,1-benzisothiazol-7-yl N-methylcarbamate (500 ppm. concentration) destroyed 100 percent of Mexican bean beetle larvae and bean aphids, four of five southern armyworms, and had no effect on two-spotted mites.

後処理

  1. customyellow solid carbamate product crystallized from solution
  2. waitto stand at room temperature overnight
  3. customsolvent and excess methylisocyanate were removed by evaporation on a rotatory evaporator
  4. washThe solid residue was washed with hot hexane
  5. customisolated by suction filtration
  6. customto give 2.6 g
  7. customyellow, microcrystalline 2,1-benzisothiazol-7-yl N-methylcarbamate, mp. 145°-148° (dec.) after recrystallization from benzene
  8. customdestroyed 100 percent of Mexican bean beetle larvae and bean aphids, four of five southern armyworms

出典と根拠

ORDレコード
ord-eeab6f83f25145f5b8349ae7d3a75d6d
出典データセット
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03997548

反応ノート

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