Dichloromethane → Ethyl 4-carbamoyloxy-4-methyl-2-pentynoate

HRID 649370노트

반응식

HRID 649370 반응식
ClCCl.[OH:4][C:5]([CH3:14])([CH3:13])[C:6]#[C:7][C:8]([O:10][CH2:11][CH3:12])=[O:9].ClS([N:19]=[C:20]=[O:21])(=O)=O>O>[C:20]([O:4][C:5]([CH3:13])([CH3:14])[C:6]#[C:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])(=[O:21])[NH2:19]

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 70918Chlorosulfonyl isocyanateHCID 112289264-Hydroxy-4-methyl-pent-2-ynoic acid ethyl ester

생성물 1

HCID 13343299Ethyl 4-carbamoyloxy-4-methyl-2-pentynoate수율 33.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 100 ml of a dichloromethane solution containing 4.9 g (31.4 millimoles) of ethyl 4-hydroxy-4-methyl-2-pentynoate, 3 ml (34.5 millimoles) of chlorosulfonyl isocyanate was added at a temperature of -10° C. The mixture was reacted for 30 minutes at -10° C. under stirring. The reaction mixture was returned to room temperature, and 20 ml of water was added thereto. The mixture was stirred for 15 minutes for hydrolysis treatment. The dichloromethane phase was separated by phase separation, washed with a 10% barium chloride solution and water successively, dried over sodium sulfate and then concentrated under reduced pressure, whereby 2.1 g (yield: 33%) of ethyl 4-carbamoyloxy-4-methyl-2-pentynoate in crystal form was obtained.

후처리

  1. additionwas added at a temperature of -10° C
  2. customThe mixture was reacted for 30 minutes at -10° C.
  3. customwas returned to room temperature
  4. stirringThe mixture was stirred for 15 minutes for hydrolysis treatment
  5. customThe dichloromethane phase was separated by phase separation
  6. washwashed with a 10% barium chloride solution and water successively
  7. dry with materialdried over sodium sulfate

출처 및 근거

ORD 기록
ord-0f1a1cf18caf4f869d4ab831ac28aa49
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04739106

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