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Triethylamine → HCID 20552969, 화합물

HRID 1446825
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HRID 1446825 반응식
[NH2:1][C:2]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].C(OCl)(C)(C)C.[CH3:23][S:24][CH2:25][C:26]([NH:28][CH3:29])=[O:27].C(N(CC)CC)C>C(Cl)Cl>[NH2:1][C:2]1[C:3]([C:4](=[O:5])[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=2)=[CH:12][C:13]([Cl:16])=[CH:14][C:15]=1[CH:25]([S:24][CH3:23])[C:26]([NH:28][CH3:29])=[O:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 128702-Amino-5-chlorobenzophenoneHCID 521297Tert-Butyl hypochloriteHCID 13553138HCID 13553138, 화합물

생성물 1

HCID 20552969HCID 20552969, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 38.3 g (0.166 mole) of 2-amino-5-chlorobenzophenone in 1 liter of methylene chloride cooled to -70° C. under an atmosphere of nitrogen was added 18.05 g (0.167 mole) of t-butylhypochlorite. The solution was stirred for 15 min and then a solution of 20.3 g (0.171 mole) of 2-methylthio-N-methylacetamide in 100 ml of methylene chloride was added. The solution was stirred at -70° C. for 2 hrs and 25 ml of triethylamine was added. While stirring, the solution was allowed to warm to room temperature followed by extraction with water and drying of the organic layer with magnesium sulfate. The volume of the solution was reduced to about 400 ml, ether was added and the solution placed in a refrigerator at about 0° C. overnight. The solid which crystallized was dried under high vacuum for about 4 hr at 50° C. Weight of the product was 31.56 g (54.6%) which melted at 170°-171° C.

후처리

  1. stirringThe solution was stirred at -70° C. for 2 hrs
  2. stirringWhile stirring
  3. extractionfollowed by extraction with water
  4. dry with materialdrying of the organic layer with magnesium sulfate
  5. additionwas added
  6. waitthe solution placed in a refrigerator at about 0° C. overnight
  7. customThe solid which crystallized
  8. customwas dried under high vacuum for about 4 hr at 50° C

출처 및 근거

ORD 기록
ord-f997dfa5412f40938ecb480c82e68ee2
출처 데이터셋
uspto-grants-1982_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04313949

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