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Water → 5-Isothiocyanato-2-(1-methyl-1H-pyrrol-2-yl)-1,3-benzoxazole

HRID 1576868
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HRID 1576868 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]([C:10]3[N:11]([CH3:15])[CH:12]=[CH:13][CH:14]=3)=[N:7][C:6]=2[CH:16]=1.[C:17](Cl)(Cl)=[S:18].C(=O)([O-])[O-].[Ca+2].O>C(Cl)(Cl)Cl>[CH3:15][N:11]1[CH:12]=[CH:13][CH:14]=[C:10]1[C:8]1[O:9][C:5]2[CH:4]=[CH:3][C:2]([N:1]=[C:17]=[S:18])=[CH:16][C:6]=2[N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 10040ThiophosgeneHCID 10112Calcium CarbonateHCID 215056582-(1-Methyl-1H-pyrrol-2-yl)-1,3-benzoxazol-5-amine

생성물 1

HCID 127819245-Isothiocyanato-2-(1-methyl-1H-pyrrol-2-yl)-1,3-benzoxazole

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

1.0 g of 5-amino-2-(1-methyl-2-pyrrolyl)benzoxazole (0.0047 mole) is dissolved in 50 ml of chloroform and slowly added to the following cold mixture: 0.54 g of thiophosgene (0.0047 mole), 0.47 g of calcium carbonate (0.0047 mole), 100 ml of chloroform and 25 ml of water. After the addition is complete the reaction is stirred at room temperature for 2 hr. The chloroform layer is separated, dried over anhyd. MgSO4 and evaporated under vacuum yielding a light brown solid. This material is crystallized from petroleum ether yielding 0.650 g of tan crystals, mp 105°-106° (54%).

후처리

  1. additionslowly added to the following cold mixture
  2. additionAfter the addition
  3. customThe chloroform layer is separated
  4. customdried over anhyd
  5. customMgSO4 and evaporated under vacuum
  6. customyielding a light brown solid
  7. customThis material is crystallized from petroleum ether yielding 0.650 g of tan crystals, mp 105°-106° (54%)

출처 및 근거

ORD 기록
ord-ef08b24cda134d4eadc0507081fb4258
출처 데이터셋
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03983130

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