Water → HCID 15010190、化合物

HRID 1033570ノート

反応式

HRID 1033570 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:9][CH:10]=[CH:11][C:12]=2[C:13]#[N:14])=[CH:4][CH:3]=1.ClS([N:19]=[C:20]=O)(=O)=O.CN(C)C=O.O>C(COC)OC>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[NH:9][C:10]([C:20]#[N:19])=[CH:11][C:12]=2[C:13]#[N:14])=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 6228DimethylformamideHCID 70918Chlorosulfonyl isocyanateHCID 146232102-(4-Chlorophenyl)-1H-pyrrole-3-carbonitrile

生成物 1

HCID 15010190HCID 15010190、化合物

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

A sample of 2-p-chlorophenyl-3-cyanopyrrole, prepared by the method of Example 4, (3.0 g, 0.015 mole) is dissolved in 50 mL of dry dimethoxyethane. To this solution is added chlorosulfonyl isocyanate (3.39 g, 0.024 mole). The addition is exothermic and some cooling is necessary. After stirring 3 hours at room temperature, dimethylformamide (6-7 mL) is added and the solution is stirred 4 hours more. The solution is then poured into water precipitating a white solid (3.4 g, 100%). A sample (1.0 g) is purified by dissolving in ethyl acetate and then passing the solution through a 60 mL course filter funnel packed with silica gel. The filtrate is concentrated to yield 0.7 g of a white solid with mp 235°-240° C.

後処理

  1. additionThe addition
  2. stirringthe solution is stirred 4 hours more
  3. customA sample (1.0 g) is purified
  4. dissolutionby dissolving in ethyl acetate
  5. filtrationfilter funnel
  6. concentrationThe filtrate is concentrated

出典と根拠

ORDレコード
ord-4435a0d361a646368dfec7e1c9288daf
出典データセット
uspto-grants-1994_05
特許番号
US05310938

反応ノート

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