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Ethanolamine → HCID 131711113, 화합물

HRID 839049
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HRID 839049 반응식
[CH2:1]([CH2:3][NH2:4])[OH:2].[SH:5][CH2:6][C:7]([NH:9][C:10]1[CH:11]=[C:12]([CH:20]=[CH:21][CH:22]=1)[C:13]([NH:15][CH2:16][C:17]([OH:19])=[O:18])=[O:14])=[O:8].C(CN(CC([O-])=O)CC(O)=O)N(CC(O)=O)CC([O-])=O.[Na+].[Na+]>O1CCCC1.O>[OH:2][CH2:1][CH2:3][NH3+:4].[SH:5][CH2:6][C:7]([NH:9][C:10]1[CH:11]=[C:12]([CH:20]=[CH:21][CH:22]=1)[C:13]([NH:15][CH2:16][C:17]([O-:19])=[O:18])=[O:14])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 700EthanolamineHCID 8759EDTA disodium saltHCID 49990HCID 49990, 화합물

생성물 1

HCID 131711113HCID 131711113, 화합물수율 93%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매3회

실험 절차

A solution 1.13 ml. of ethanolamine (1.15 g., 0.0188 mole) and 10 ml. of tetrahydrofuran is added to a suspension of N-[3-(mercaptoacetylamino)benzoyl]glycine (5 g., 0.0186 mole), 5 mg. of disodium edetate, 6 ml. of water, and 40 ml. of tetrahydrofuran. Warming the mixture to 40°-45° C. provides a clear solution which is first diluted with 200 ml. of tetrahydrofuran, then cooled in a dry ice-acetone bath to promote crystallization and subsequently stirring for a period of 16 hrs. at room temperature. The precipitated material formed is collected, washed with tetrahydrofuran and dried over calcium chloride to afford 5.7 g., (93% yield) of N-[3-(mercaptoacetylamino)benzoyl]glycine 2-hydroxyethyl ammonium salt, m.p. 144.0°-160.0° C. (dec.).

후처리

  1. temperatureWarming the mixture to 40°-45° C.
  2. customprovides a clear solution which
  3. additionis first diluted with 200 ml
  4. customcrystallization
  5. customat room temperature
  6. customThe precipitated material formed
  7. customis collected
  8. washwashed with tetrahydrofuran
  9. dry with materialdried over calcium chloride
  10. customto afford 5.7 g

출처 및 근거

ORD 기록
ord-41c6c68b7b584086818f8434d7f2faf9
출처 데이터셋
uspto-grants-1978_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04093739

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