Bromine → N6-propyl-4,5,6,7-tetrahydro-benzothiazole-2,6-diamine dihydrobromide

HRID 1942385ノート

反応式

HRID 1942385 の反応式
O1[C:5]2([CH2:10][CH2:9][CH:8]([NH:11][CH2:12][CH2:13][CH3:14])[CH2:7][CH2:6]2)OCC1.[Br:15]Br.[NH2:17][C:18]([NH2:20])=[S:19]>Br>[BrH:15].[BrH:15].[CH2:12]([NH:11][CH:8]1[CH2:9][CH2:10][C:5]2[N:17]=[C:18]([NH2:20])[S:19][C:6]=2[CH2:7]1)[CH2:13][CH3:14]

参加物

5

反応物 3

HCID 24408BromineHCID 2723790ThioureaHCID 118200814-n-Propylamino-cyclohexanone-ethyleneketal

生成物 1

HCID 86651296N6-propyl-4,5,6,7-tetrahydro-benzothiazole-2,6-diamine dihydrobromide

試薬・触媒・溶媒 1

HCID 260Hydrogen Bromide溶媒

実験手順

A solution of 12.0 g (60 mmol) (1,4-dioxa-spiro[4.5]dec-8-yl)-propyl-amine in 120 mL concentrated aqueous hydrobromic acid is stirred for 15 minutes at room temperature and then 3.12 mL (60 mmol) bromine are added. After further stirring for 15 minutes 4.56 g (60 mmol) of thiourea is added. The resulting solution is stirred for another at room temperature until a white precipitation can be observed. Afterwards the mixture is heated for 2 hours at 90° C. The clear reaction mixture is then concentrated under vacuum. The solid residue is suspended in ethanol, heated to reflux and filtrated after cooling to room temperature. The resulting residue is dried under high vacuum.

後処理

  1. additionis added
  2. customuntil a white precipitation
  3. temperatureAfterwards the mixture is heated for 2 hours at 90° C
  4. concentrationThe clear reaction mixture is then concentrated under vacuum
  5. temperatureheated
  6. temperatureto reflux
  7. filtrationfiltrated
  8. temperatureafter cooling to room temperature
  9. customThe resulting residue is dried under high vacuum

出典と根拠

ORDレコード
ord-90fff8bf885c418a965e52181c1bfc5a
出典データセット
uspto-grants-2013_03
特許番号
US08389555B2

反応ノート

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