Bromine → HCID 13340370, 화합물

HRID 2052471노트

반응식

HRID 2052471 반응식
[NH2:1][C:2]1[CH:17]=[CH:16][CH:15]=[CH:14][C:3]=1[CH2:4][NH:5][C@H:6]([C:11]([OH:13])=[O:12])[CH2:7][CH2:8][S:9][CH3:10].[Cl-].[Al+3].[Cl-].[Cl-].[Br:22]Br>C(O)(=O)C>[NH2:1][C:2]1[CH:17]=[CH:16][C:15]([Br:22])=[CH:14][C:3]=1[CH2:4][NH:5][C@H:6]([C:11]([OH:13])=[O:12])[CH2:7][CH2:8][S:9][CH3:10]

참가 물질

5

반응물 3

HCID 24408Bromine2회HCID 6451240Aluminum(III) ChlorideHCID 13340364N-[(2-Aminophenyl)methyl]-L-methionine

생성물 1

HCID 13340370HCID 13340370, 화합물수율 45%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

2.54 gm (0.01 mol) of N-(2-amino-benzyl)-methionine and 100 gm of aluminum chloride were dissolved in 50 cc of anhydrous acetic acid while gently heating. Then, the mixture was brought to room temperature and, while stirring, 0.52 cc (0.01 mol) of bromine diluted in 20 cc of acetic acid was added slowly. A light-colored precipitate was formed. After the addition of bromine was finished, the precipitate was centrifuged off, washed with ample acetic acid and then with anhydrous ether, and dried in a dryer. Then, the product was dissolved in 40 cc of water, and the pH of the solution was adjusted to 6 by addition of dilute ammonia while cooling it on an ice water bath. The mixture was allowed to stand for 24 hours, whereupon the new precipitate was centrifuged off, washed with water and dried in drying chamber. (Solvent of the crystallizate: alcohol at 50° C.). The melting point of the product was 207° C., and the yield was 45% of theory.

후처리

  1. temperaturewhile gently heating
  2. customwas brought to room temperature
  3. additionwas added slowly
  4. customA light-colored precipitate was formed
  5. washwashed with ample acetic acid
  6. dry with materialwith anhydrous ether, and dried in a dryer
  7. dissolutionThen, the product was dissolved in 40 cc of water
  8. additionthe pH of the solution was adjusted to 6 by addition of dilute ammonia
  9. temperaturewhile cooling it on an ice water bath
  10. washwashed with water
  11. customdried
  12. customin drying chamber
  13. customat 50° C.
  14. customwas 207° C.

출처 및 근거

ORD 기록
ord-9258067c1cdb4ef1a29429ae6fb9ac5f
출처 데이터셋
uspto-grants-1980_01
특허 번호
US04185114

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