Dichloromethane → Methyl 8-cyano-2-[(2,2-diethoxyethyl)sulfanyl]octanoate

HRID 1678926ノート

反応式

HRID 1678926 の反応式
Br[CH:2]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]#[N:14])[C:3]([O:5][CH3:6])=[O:4].[CH2:15]([O:17][CH:18]([O:21][CH2:22][CH3:23])[CH2:19][SH:20])[CH3:16].C(Cl)Cl>C(N(CC)CC)C>[CH2:15]([O:17][CH:18]([O:21][CH2:22][CH3:23])[CH2:19][S:20][CH:2]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]#[N:14])[C:3]([O:5][CH3:6])=[O:4])[CH3:16]

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 109426222,2-diethoxy-ethanethiolHCID 20364819Methyl 2-bromo-8-cyanooctanoate

生成物 1

HCID 54422104Methyl 8-cyano-2-[(2,2-diethoxyethyl)sulfanyl]octanoate

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

The starting material is prepared as follows: To the mixture of 13.6 g of methyl 2-bromo-8-cyano-octanoate, 11.6 g of 2,2-diethoxy-ethylmercaptan and 150 ml of methylene chloride, 5.56 g of triethylamine are added dropwise while stirring. After overnight-stirring at room temperature the mixture is evaporated, the residue triturated with diethyl ether, washed with water, dried and evaporated, to yield the methyl 2-(2,2-diethoxyethylmercapto)-8-cyano-octanoate showing NMR bands at 4.58, 3.71 and 2.75 ppm.

後処理

  1. customThe starting material is prepared
  2. additionare added dropwise
  3. stirringAfter overnight-stirring at room temperature the mixture
  4. customis evaporated
  5. customthe residue triturated with diethyl ether
  6. washwashed with water
  7. customdried
  8. customevaporated

出典と根拠

ORDレコード
ord-aefe63b3a56641248ab51f8c7cce7dca
出典データセット
uspto-grants-1978_03
特許番号
US04077979

反応ノート

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