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Thiophosgene → HCID 13563671, 화합물

HRID 979720
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HRID 979720 반응식
[C:1]([C:5]1[CH:6]=[C:7]([OH:12])[CH:8]=[CH:9][C:10]=1[Cl:11])([CH3:4])([CH3:3])[CH3:2].[C:13](Cl)([Cl:15])=[S:14].[OH-].[Na+]>C(Cl)(Cl)Cl>[Cl:15][C:13]([O:12][C:7]1[CH:8]=[CH:9][C:10]([Cl:11])=[C:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[CH:6]=1)=[S:14]
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참가 물질

5

반응물 3

HCID 10040ThiophosgeneHCID 14798Sodium HydroxideHCID 109102303-Tert-butyl-4-chlorophenol

생성물 1

HCID 13563671HCID 13563671, 화합물수율 72.5%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Into 50 ml of chloroform were dissolved 9.2 g of 3-tert-butyl-4-chlorophenol and 6.3 g of thiophosgene, and 60 ml of 1N-sodium hydroxide solution were added dropwise thereto with stirring at room temperature. After completion of this dropwise addition, the mixture was subjected to stirring over a period of 3 hours. From the reaction mixture was separated chloroform layer, which was thereafter dried over anhydrous calcium chloride. Then, chloroform was distilled off and the residue was distilled under reduced pressure to give 9.5 g of O-3-tert-butyl-4-chlorophenyl chlorothioformate having boiling point of 103°-106° C./0.5 mmHg, of which properties are as follows.

후처리

  1. additionwere added dropwise
  2. additionAfter completion of this dropwise addition
  3. stirringto stirring over a period of 3 hours
  4. customFrom the reaction mixture was separated chloroform layer, which
  5. dry with materialwas thereafter dried over anhydrous calcium chloride
  6. distillationThen, chloroform was distilled off
  7. distillationthe residue was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-7e9adeac2b2140798021751f2df1614a
출처 데이터셋
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04668831

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