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Carbon Disulfide → HCID 13302038、化合物

HRID 620071
ノート
印刷プレビュー

反応式

HRID 620071 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

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

生成物 1

HCID 13302038HCID 13302038、化合物

試薬・触媒・溶媒 3

HCID 679Dimethyl Sulfoxide溶媒
HCID 962
Water
溶媒
2 回
HCID 8058Hexane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-9cbdcc59e38a4bb29c849cc2de21e66c
出典データセット
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04818765

反応ノート

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