Methyl chloroformate → HCID 178502040、化合物

HRID 838995ノート

反応式

HRID 838995 の反応式
S(O)(O)(=O)=O.CS[C:8](=[NH:10])[NH2:9].Cl[C:12]([O:14][CH3:15])=[O:13].[OH-].[Na+].[Cl:18][C:19]1([Cl:32])[CH2:21][CH:20]1[CH2:22][S:23][C:24]1[CH:29]=[CH:28][C:27]([NH2:30])=[C:26](N)[CH:25]=1>O.CO.C(O)(=O)C>[Cl:32][C:19]1([Cl:18])[CH2:21][CH:20]1[CH2:22][S:23][C:24]1[CH:29]=[CH:28][C:27]2[NH:30][C:8]([NH:9][C:12](=[O:13])[O:14][CH3:15])=[N:10][C:26]=2[CH:25]=1

参加物

8

反応物 4

HCID 6586Methyl chloroformateHCID 14798Sodium HydroxideHCID 752702-Methyl-2-thiopseudourea sulfateHCID 20532837HCID 20532837、化合物

生成物 1

HCID 178502040HCID 178502040、化合物

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a mixture of 9 g of 2-methyl-2-thiopseudourea sulfate in 6 ml of H2O there is added 5.7 ml of methyl chloroformate at 0° C and the mixture is stirred for 15 minutes. Then there is added 12 ml of 25% NaOH dropwise and the mixture is stirred for 15 minutes. Then there is added 6 ml of acetic acid dropwise and the mixture is stirred for 15 minutes. Then the total amount of 4-[(2,2-dichlorocyclopropyl)methyl]thio-o-phenylenediamine from above in 50 ml of methanol is added and the mixture is refluxed for 2 hours. The alcohol is removed in vacuo and H2O is added. The resulting solid is filtered off and crystallized from glyme to yield 5.4 g, m.p. 211-213°.

後処理

  1. stirringthe mixture is stirred for 15 minutes
  2. stirringthe mixture is stirred for 15 minutes
  3. temperaturethe mixture is refluxed for 2 hours
  4. customThe alcohol is removed in vacuo and H2O
  5. additionis added
  6. filtrationThe resulting solid is filtered off
  7. customcrystallized from glyme
  8. customto yield 5.4 g, m.p. 211-213°

出典と根拠

ORDレコード
ord-31e8a5fa773f451c874040e52d18167b
出典データセット
uspto-grants-1978_06
特許番号
US04093732

反応ノート

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