Hydrazine hydrate (1:1) → Cyclohexanecarboxylic acid, 2-hydroxy-, hydrazide, trans-(9CI)

HRID 1823662노트

반응식

HRID 1823662 반응식
[OH:1][C@@H:2]1[CH2:7][CH2:6][CH2:5][CH2:4][C@H:3]1[C:8]([O:10]CC)=O.O.[NH2:14][NH2:15]>CC(O)C>[OH:1][C@@H:2]1[CH2:7][CH2:6][CH2:5][CH2:4][C@H:3]1[C:8]([NH:14][NH2:15])=[O:10]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 1268212trans-Ethyl 2-hydroxycyclohexanecarboxylate

생성물 1

HCID 14687012Cyclohexanecarboxylic acid, 2-hydroxy-, hydrazide, trans-(9CI)수율 32%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

To a one-liter four-necked flask were added 102.5 g (595 mmol) of ethyl (R,R)-2-hydroxycyclohexanecarboxylate and 400 mL of 2-propanol and stirring was started. Hydrazine monohydrate (44.7 g; 893 mmol) was dropped thereinto at 13° C. taking 30 minutes. After the dropping, the mixture was stirred at 80° C. for 9.5 hours. Followed by, heating was stopped and the mixture was cooled to room temperature to precipitate the crystals. The crystals were filtered and washed with a small amount of 2-propanol. The resulting crystals were dried to give 30.10 g of the title compound. The yield was 32%.

후처리

  1. stirringAfter the dropping, the mixture was stirred at 80° C. for 9.5 hours
  2. temperatureFollowed by, heating
  3. customto precipitate the crystals
  4. filtrationThe crystals were filtered
  5. washwashed with a small amount of 2-propanol
  6. customThe resulting crystals were dried

출처 및 근거

ORD 기록
ord-01befda9e3904bf3a8a174f537bdd9df
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07038087B2

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