Accelerator DM → HCID 53841864、化合物

HRID 370125

反応式

HRID 370125 の反応式
ClCl.S1C2C=CC=CC=2N=[C:4]1[S:12][S:13][C:14]1[S:15][C:16]2[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=2[N:18]=1.S[CH2:24][CH:25]([OH:27])C>ClC1C=CC=CC=1>[OH:27][CH:25]([CH3:24])[CH2:4][S:12][S:13][C:14]1[S:15][C:16]2[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=2[N:18]=1

参加物

5

反応物 3

HCID 8447Accelerator DMHCID 24526ChlorineHCID 1025451-Mercapto-2-propanol

生成物 1

HCID 53841864HCID 53841864、化合物収率 146.1%

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

実験手順

Chlorine gas (17.5 g/0.25 mole) was passed at 0 to 5° C. into a suspension of 2,2'-dithiobisbenzthiazole (83 g/0.25 mole) in chlorobenzene (600 ml). 1-mercapto-2-propanol (46 g/0.5 mole) was then added drop-wise to this solution, followed by stirring for 7 hours at room temperature. The precipitated product was filtered off and mixed with methylene chloride (500 ml) and 5% NaHCO3 solution (500 ml). The organic phase was then washed twice with water and concentrated by evaporation. A yellowish-brown oil (94 g) was obtained.

後処理

  1. filtrationThe precipitated product was filtered off
  2. additionmixed with methylene chloride (500 ml) and 5% NaHCO3 solution (500 ml)
  3. washThe organic phase was then washed twice with water
  4. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-1a57b3f6f510468a8777d861b0faa4fa
出典データセット
uspto-grants-2000_10
特許番号
US06140427

関連ノート

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