Dichloromethane → HCID 380419、化合物

HRID 1645407ノート

反応式

HRID 1645407 の反応式
C1C=CC(S(N(S(C2C=CC=CC=2)(=O)=O)[F:11])(=O)=O)=CC=1.[H-].[Na+].[CH2:23]1[S:31](=[O:33])(=[O:32])[O:30][CH2:29][CH2:28][O:27][S:24]1(=[O:26])=[O:25].C(Cl)Cl>O1CCCC1.C(#N)C>[F:11][CH:23]1[S:24](=[O:25])(=[O:26])[O:27][CH2:28][CH2:29][O:30][S:31]1(=[O:33])=[O:32]

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 24758Sodium hydrideHCID 57513CyclodisoneHCID 588007N-Fluorobenzenesulfonimide2 回

生成物 1

HCID 380419HCID 380419、化合物

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

The fluorinating agent used was N-fluorobenzenesulfonimide obtained from PCR Chemicals (Gainesville Fla.). To a suspension of 0.34 g of NaH in 50 mL of tetrahydrofuran was added 2.45 g of ethylene methanedisulfonate followed by 3.8 g of N-fluorobenzenesulfonimide in 25 mL of acetonitrile. After about 15 min, 25 mL of CH2Cl2 was added, the solution was filtered, and the product was isolated by crystallization from CH2Cl2-cyclohexane to give 0.49 g of ethylene fluoromethanedisulfonate, m.p. 84-86° C. (93-2).

後処理

  1. customobtained from PCR Chemicals (Gainesville Fla.)
  2. filtrationthe solution was filtered
  3. customthe product was isolated by crystallization from CH2Cl2-cyclohexane

出典と根拠

ORDレコード
ord-663e47e8dd484e81975b9818f0c8529a
出典データセット
uspto-grants-2012_02
特許番号
US08124793B2

反応ノート

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