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Acetonitrile → 7-Iodobenzofuran-5-sulfonyl chloride

HRID 1162035
ノート
印刷プレビュー

反応式

HRID 1162035 の反応式
CC(N=NC(C#N)(C)C)(C#N)C.C1C(=O)N(Br)C(=O)C1.[I:21][C:22]1[C:30]2[O:29][CH2:28][CH2:27][C:26]=2[CH:25]=[C:24]([S:31]([Cl:34])(=[O:33])=[O:32])[CH:23]=1.C(#N)C>ClC1C=CC=CC=1>[I:21][C:22]1[C:30]2[O:29][CH:28]=[CH:27][C:26]=2[CH:25]=[C:24]([S:31]([Cl:34])(=[O:32])=[O:33])[CH:23]=1
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 6342AcetonitrileHCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 534309327-Iodo-2,3-dihydrobenzofuran-5-sulfonyl chloride2 回

生成物 1

HCID 534029757-Iodobenzofuran-5-sulfonyl chloride収率 90%

試薬・触媒・溶媒 1

HCID 7964
Chlorobenzene
溶媒

実験手順

AIBN (270 mg, 1.3 mmol) and NBS (2.5 g, 14 mmol) were added to 7-iodo-2,3-dihydro-benzofuran-5-sulfonyl chloride (4.4 g, 13 mmol; Intermediate 55) in chlorobenzene (30 mL) at 70° C. The heating was turned off one hour after the addition. Acetonitrile (30 mL) was added and the organic phase was washed with sodium sulphite in water. The organic phase was separated and the volatiles were evaporated to give 4 g (90%) of the title compound as yellow crystals. 1H NMR 270 MHz (CDCl3) δ ppm 7.07 (d, J=2.23 Hz, 1H) 7.90 (d, J=2.23 Hz, 1H) 8.29-8.37 (m, 1H).

後処理

  1. additionafter the addition
  2. washthe organic phase was washed with sodium sulphite in water
  3. customThe organic phase was separated
  4. customthe volatiles were evaporated

出典と根拠

ORDレコード
ord-65685197f9e04014aba6dfbd8b3a05a6
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07820675B2

反応ノート

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