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Water → 5-(1,1-Dimethylethyl)-7-iodo-1,2-benzisoxazole

HRID 263038
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HRID 263038 반응식
[CH3:1][C:2]([C:5]1[CH:13]=[C:9]([CH:10]=[N:11]O)[C:8]([OH:14])=[C:7]([I:15])[CH:6]=1)([CH3:4])[CH3:3].ClC(Cl)(Cl)C(N=C=O)=O.C(=O)([O-])[O-].[K+].[K+].O>O1CCCC1>[CH3:1][C:2]([C:5]1[CH:6]=[C:7]([I:15])[C:8]2[O:14][N:11]=[CH:10][C:9]=2[CH:13]=1)([CH3:4])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 76400Trichloroacetyl isocyanateHCID 1363987985-(1,1-Dimethylethyl)-3-iodosalicylaldoxime

생성물 1

HCID 130475665-(1,1-Dimethylethyl)-7-iodo-1,2-benzisoxazole수율 46.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 3.19 g of 5-(1,1-dimethylethyl)-3-iodosalicylaldoxime in 10 ml of tetrahydrofuran is added 2.0 g of trichloroacetylisocyanate in tetrahydrofuran (5 ml) at room temperature followed by addition of 1.52 g of potassium carbonate. The mixture is stirred for an additional 20 minutes before it is poured into 400 ml of water. The precipitate so obtained is crystallized from methanol to afford 1.4 g (46.5%) of 5-(1,1-dimethylethyl)-7-iodo-1,2-benzisoxazole, m.p. 106°-109° C.

후처리

  1. customThe precipitate so obtained
  2. customis crystallized from methanol

출처 및 근거

ORD 기록
ord-4ef0f1efa6db46ca83aaf7911f08e45f
출처 데이터셋
uspto-grants-1979_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04156005

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