Triethylamine → [1,1':3', 1"-Terphenyl]-2'-yl[[[2,6-bis(1-methylethyl)phenyl]amino]sulfonyl]carbamat

HRID 1742033ノート

反応式

HRID 1742033 の反応式
[C:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:8]=2[O:19][C:20](=[O:26])[NH:21][S:22](Cl)(=[O:24])=[O:23])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:27]([C:30]1[CH:36]=[CH:35][CH:34]=[C:33]([CH:37]([CH3:39])[CH3:38])[C:31]=1[NH2:32])([CH3:29])[CH3:28].C(N(CC)CC)C>O1CCCC1>[C:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:8]=2[O:19][C:20](=[O:26])[NH:21][S:22]([NH:32][C:31]2[C:33]([CH:37]([CH3:38])[CH3:39])=[CH:34][CH:35]=[CH:36][C:30]=2[CH:27]([CH3:29])[CH3:28])(=[O:24])=[O:23])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 32484DiisopropylanilineHCID 10572313[1,1':3',1"-Terphenyl]-2'-yl(chlorosulfonyl)carbamate

生成物 1

HCID 10506346[1,1':3', 1"-Terphenyl]-2'-yl[[[2,6-bis(1-methylethyl)phenyl]amino]sulfonyl]carbamat

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of [1,1':3', 1"-terphenyl]-2'-yl(chlorosulfonyl)carbamate (5.0 g, 12.9 mmol) in 75 mL tetrahydrofuran was added dropwise to a solution of 2,6-diisopropyl aniline (2.29 g, 12.9 mmol) and triethylamine (1.3 g, 12.9 mmol) in 100 mL tetrahydrofuran at -15° C. under an atmosphere of nitrogen. The resulting mixture was warmed to room temperature and stirred for 16 hours. Concentrated in vacuo and partitioned the residue between water and ethyl acetate. Dried the organic layer over MgSO4 and evaporated to give an off-white solid. Chromatography on silica gel gave the title compound, mp 166°-168° C.

後処理

  1. concentrationConcentrated in vacuo
  2. custompartitioned the residue between water and ethyl acetate
  3. dry with materialDried the organic layer over MgSO4
  4. customevaporated
  5. customto give an off-white solid

出典と根拠

ORDレコード
ord-f09b8a53804a4aa4abd7076939c4f1b7
出典データセット
uspto-grants-1994_08
特許番号
US05336690

反応ノート

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