Bromine → 2-Amino-6-benzylbenzothiazole

HRID 9125

반응식

HRID 9125 반응식
[CH2:1]([C:8]1[CH:14]=[CH:13][C:11]([NH2:12])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:15]([S-:17])#[N:16].[K+].BrBr>C(O)(=O)C>[NH2:16][C:15]1[S:17][C:13]2[CH:14]=[C:8]([CH2:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[CH:9]=[CH:10][C:11]=2[N:12]=1

참가 물질

5

반응물 3

HCID 24408BromineHCID 136914Benzenamine, 4-(phenylmethyl)-HCID 516872Potassium thiocyanate

생성물 1

HCID 219855102-Amino-6-benzylbenzothiazole수율 88.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

A solution of 4-benzylaniline (0.916 g, 5.00 mmol) and KSCN (0.97 g, 10.0 mmol, 2.0 eq) in 10 mL acetic acid was cooled at about 5° C., and was treated dropwise with a solution of bromine (0.258 mL, 5.00 mmol, 1.0 eq) in 2 mL acetic acid. The mixture was stirred at room temperature for about 1 hour. The precipitate was filtered off and washed with Et2O. The obtained solid was neutralized with saturated sodium carbonate solution, and a new precipitate was formed. It was filtered off, washed with water and MeOH, and dried under vacuum to give the desired compound 1.06 g (88%). LC/MS 241.2 (M+1); LC retention time 2.46 min.

후처리

  1. filtrationThe precipitate was filtered off
  2. washwashed with Et2O
  3. customa new precipitate was formed
  4. filtrationIt was filtered off
  5. washwashed with water and MeOH
  6. customdried under vacuum

출처 및 근거

ORD 기록
ord-74007a0173b8457e84bcfc9f8de348a6
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091227B2

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