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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Carbon Disulfide → HCID 13302038, 화합물

HRID 1709006
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HRID 1709006 반응식
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:4]=[C:5]([CH2:9][C:10]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])=[O:11])[CH:6]=[CH:7][CH:8]=1.[C:23](=[S:25])=[S:24].[OH-].[K+].Cl[CH2:29][CH2:30][CH2:31]Cl>CS(C)=O.O.CCCCCC>[S:24]1[CH2:31][CH2:30][CH2:29][S:25][C:23]1=[C:9]([C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:21])([F:22])[F:1])[CH:4]=1)[C:10]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 6348Carbon DisulfideHCID 88811,3-DichloropropaneHCID 14797Potassium HydroxideHCID 13302037Octyl [3-(trifluoromethyl)phenyl]acetate

생성물 1

HCID 13302038HCID 13302038, 화합물

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매
HCID 962
Water
용매
2회
HCID 8058Hexane용매

실험 절차

To a solution of n-octyl 3-trifluoromethylphenylacetate (112.2 g) in dimethyl sulphoxide (850 ml) there are added carbon disulphide (30.4 g) and, slowly, a solution of potassium hydroxide (60.0 g) in water (100 ml). The mixture is stirred for 2 hours at 40°. 1,3-dichloropropane (40.1 g) is then added and the mixture is stirred at 50° for 3 hours. Water (800 ml) and hexane (800 ml) are added, the two phases are separated and the aqueous solution is extracted with hexane (2×500 ml). The combined organic phases are washed with water (400 ml), dried over magnesium sulphate and evaporated. The residue is crystallized from pentane. The product is dried in vacuo to constant weight to yield n-octyl (1,3-dithian-2-ylidene)-(3-trifluoromethylphenyl)-acetate, m.p. 49° (as Example 11).

후처리

  1. stirringthe mixture is stirred at 50° for 3 hours
  2. customthe two phases are separated
  3. extractionthe aqueous solution is extracted with hexane (2×500 ml)
  4. washThe combined organic phases are washed with water (400 ml)
  5. dry with materialdried over magnesium sulphate
  6. customevaporated
  7. customThe residue is crystallized from pentane
  8. customThe product is dried in vacuo to constant weight

출처 및 근거

ORD 기록
ord-c92aa8d19d8b4825a550506975fc81dc
출처 데이터셋
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04946861

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